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Page 1: Durham E-Theses Aspects of structure and functionality in

Durham E-Theses

Aspects of structure and functionality in legumin and

vicilin from vicia faba seeds

Cully, Julia

How to cite:

Cully, Julia (1987) Aspects of structure and functionality in legumin and vicilin from vicia faba seeds,Durham theses, Durham University. Available at Durham E-Theses Online: http://etheses.dur.ac.uk/6713/

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Academic Support O�ce, Durham University, University O�ce, Old Elvet, Durham DH1 3HPe-mail: [email protected] Tel: +44 0191 334 6107

http://etheses.dur.ac.uk

Page 2: Durham E-Theses Aspects of structure and functionality in

ASPECI'S OF srRUCI'URE AND FUNcriONALITY IN LEGlMIN AND VICILIN FRCM VICIA FABA

SEEDS.

BY

JULIA a.JLLY

A thesis submitted 1n fulfilment of the requirements· for the degree of

Doctor of Philosophy

to

THE UNIVERSITY OF DURHAM

The copyright of this thesis rests with the author.

No quotation from it should be published without

his prior written consent and information derived

DEPARIMENT OF BarANY, UNIVERSITY OF DURHAM.

from it should be acknowledged.

-h .lUI !987

JANUARY 1987

Page 3: Durham E-Theses Aspects of structure and functionality in

DECLARATION

I declare that no part of this thesis has previously

been subnutted for a degree at this or any other

University. Also, that the work presented in this

thesis is entirely my own.

The copyright of this thesis rests with the author.

No quotation from it should be published without her

prior written consent, and Information derived from

1t should be acknowledged.

Page 4: Durham E-Theses Aspects of structure and functionality in

ABSTRA.Cr.

Cully, J.

Aspects of structure and functionality in legumin and v1c1l1n

from V1c1a faba seeds.

Soy beans command a large proport1on of the vegetable prote1n

market of the food process1ng 1ndustry; however, the1r cult1vat1on 1s

llm1ted by cllmat1c factors. A crop able to compete in these IIICIIkets,

but su1ted to growth 1n cooler, temperate cond1t1ons would have

pollt1cal and econom1c advantages for Europe. One such crop under

cons1deration 1s V1c1a faba m1nor. A new faba bean llne ( IVS-G) ,

developed by a breed1ng programme at Durham Un1vers1ty, was compared

to an establlshed commerc1al var1ety (Marls Bead) for chem1cal,

phys1cal and funct1onal character1st1cs. A select1on of processing

methods was used to produce prote1naceous mater1als equivalent to soy

products already on the COIIUilerclal market. The methOO.s used were

defatt1ng, a1r-class1ficat1on, and the prOO.uction of 1solates,

prote1nates and micellar prote1n preparat1ons. The mater1als were

assessed and compared to soy prOO.ucts for funct1onal1ty 1n tests

des1gned to assess solub1l1ty, gell1ng, foam1ng and emuls1fy1ng

propert1es. The storage prote1ns, legum1n and Vlcllln, are the maJor

prote1n const1tuents of the bean seed, and the1r structural and

functional propert1es were also 1nvest1gated.

The bean products had similar funct1onal propert1es to

equ1valent soy products, when prote1n contents were also Slmilar.

Ha.·1ever, the hlgher 1n1t1al 1n v1vo prote1n content of the soy bean

does g1ve the latter a oompet1t1ve advantage. Also, the market1ng of

by-products of faba bean, eg. starch and f1bre, may prove difflcult.

I

Page 5: Durham E-Theses Aspects of structure and functionality in

Abbrev1at1ons

BSA bov1ne serum album1n

CWM cell wall material

DSC d1fferent1al scann1ng calor1metry

DTI' d1th1othr1e1tol

EDI'A - ethylened1am1ne tetraacetate

PAGE polyacrylam1de gel electrophores1s

PSE prote1n separat1on eff1c1ency

py prote1n y1eld

SAXS small angle X-ray scatter1ng

SDS scxhum dodecyl sulphate

S.EM scann1ng electron m1croscopy

SSE starch separat1on eft1c1ency

SY starch y1eld

Tr1s tr1s(hydroxymethyl)am1nomethane

11

Page 6: Durham E-Theses Aspects of structure and functionality in

Contents

Page Nwnber

Abstract

Abbreviations

Contents

i

ii

ill

List

List

1.0

2.0

3.0

of tables

of flgures

INTRO.cucrioo

MATERIALS

2.1 Biological materials

2.2 Chemicals and reagents

2.3 Other materials

METHOI'S

3.1 Preparation of experimental material

VI

VIII

1

16

17

17

3.1.1 Preparation of flour for air-classification 18

3.1.2 Preparation ot flour for protein purification 18

3.2 Fractionation of flours

3.2.1 ~r-classification

3.2.2 Re-classification of coarse fraction

3.2.3 Sequential air-classification

3.2.4 Protein yield, protein separation efficiency,

18

19

19

starch yield and starch separation efficiency 19

3.3 Analysis of flours amd air-classified fractions

3.3.1 Moisture content deterffilnation

3.3.2 Protein determination

3.3.3 Starch deterffilnation

3.4 Isolate, proteinate and micellar protein production

3.4.1 Isolate preparation

3.4.2 Proteinate preparation

111

20

20

21

21

21

Page 7: Durham E-Theses Aspects of structure and functionality in

3.4.3 M1cellar prote1n preparation 21

3.5 Pur1ficat1on of storage prote1ns

3.5.1 crude extract1on of storage prote1ns 22

3.5.2 Separation of crude globulins on HA-Ultrogel 23

3.6 Analys1s of prote1ns

3.6.1 Polyacrylamide gel electrophores1s (PAGE) 23

3.6.2 Analysis of pur1f1ed prote1ns on Superose 6 24

3.6.3 Analyt1cal ultracentr1fugat1on 24

3.7 Measurement of solub1l1ty and gelling ab1l1ty

3.7.1 Measurement of solub1l1ty and gell1ng abil1ty

as a funct1on of pH 25

3.7.2 Assessment of gell1ng propert1es by a

compress1.on

measurements

test and

3.8 Assessment of foarn1.ng abllity

stress relaxat1on

3.8.1 Determ1nat1.on of foarn1ng ab1.l1.ty by a

large-scale wh1pp1.ng method

3.8.2 Deterrn1nat1.on of foarn1ng ability by a

small-scale sparg1ng method

3.8.3 Compar1.son of wh1pp1.ng and sparg1.ng methods

26

28

30

for determ1.n1.ng foarn1ng properties 32

3.8.4 Invest1.gat1.on of the effect of sucrose on

foarn1ng propert1.es

3.9 Deterrn1nation of ernuls1.on act1.v1.ty

3.10 Dlfferential scann1.ng calor1.metry

3.11 Scann1.ng electron m1.croscopy

4.0 RESULTS

4.1 Alr-class1.f1.cat1.on and analys1.s of flours

4.2 Evaluat1.on of 1.solates, prote1.nates and m1.cellar

prote1.ns

l.V

33

33

33

34

35

50

Page 8: Durham E-Theses Aspects of structure and functionality in

4.3 Purif1cat1on and analys1s of prote1ns 53

4.4 D1spers1b1lity and gelling character1st1cs of

1solates, prote1nates and m1cellar prote1ns

4.5 Assessment of foam1ng abil1ty

4.6 Assessment of emuls1on act1v1ty

4.7 Dlfferential scann1ng calor1metry

5.0 DISaJSSICN

6. 0 REFERENCES

Acknowledgements

v

59

79

97

101

104

156

177

Page 9: Durham E-Theses Aspects of structure and functionality in

List of Tables

Page Number

Table l. M01.sture, prote1n and starch contents of Marls

Bead and IVS-G flours. 35

Table 2. Air-class1ficat1on of Marls Bead and IVS-G flours. 36

Table 2a. A.u-classificatlon of IVS-G flours subJected to a

second pass through a Kolloplex m1ll. 36

Table 3. Percentage protein of a1r-class1f1ed fractions of

Marls Bead and IVS-G flours. 37

Table 3a. Percentage protein of a1r-class1fied fractions of

IVS-G flours subJected to a second _pa.ss through a

Kolloplex mlll. 37

Table 4. Percentage starch of a1r-class1f1ed tract1ons of

Marls Bead and IVS-G flours. 39

Table 5. Proteln y1elds and prote1n separat1on eff1cienc1es

of a1r-class1f1ed

IVS-G flours.

fract1ons of Marls Bead and

Table Sa. Proteln y1elds and prote1n separat1on eff1c1enc1es

of a1r-class1f1ed fract1ons of IVS-G flours

subJected to a second _pa.ss through a Kolloplex

m1ll.

Table 6. Starch y1elds and starch separation eff1c1enc1es

of a1r-class1f1ed tract1ons of Mar1s Bead and

IVS-G flours.

Table 7. Y1eld and content of prote1n and starch

concentrates produced by reclass1f1cat1on of the

40

40

41

coarse fract1on obta1ned at 6500 rev./m1n. 46

Table 8. Sequent1al class1hcat1on of Marls Bead and IVS-G

flours. 47

Vl

Page 10: Durham E-Theses Aspects of structure and functionality in

Table 9. Percentage protein in sequentially classified

fract1.ons of Mans Bead and IVS-G flours. 48

Table 10. Protein contents of 1.solates, proteinates and

m1.cellar proteins. 53

Table 11. 8ed1mentation coefficients of 118 and 78 prote1.ns. 56

Table 12. Uniax1al compress1.oo of 1.solate, proteinate and

micellar protein gels. 74

Table 13. Protel.n cootents of 20% solutl.ons prior to gelling. 75

Table 14. Relaxation times of isolate, protel.nate and

m1.cellar protel.n gels. 77

Table 15. Co-ordinatl.on number of the f1rst flow process 1.n

gels subJected to stress-relaxation experiments. 78

Table 16. Foam1.ng abill. ty from whipping and sparging

exper1.ments. 80

Table 17. compar1.son of wh1pp1ng and sparg1.ng methods for

determ1.ning foam expansion and foam stabl.lity. 96

Table 18. The effect of sucrose oo the foam1.ng ability of a

defatted Marl.s Bead prote1.nate. 99

Table 19. Emuls1.on act1.v1.ties of flours, concentrates,

1.solates, proteinates, and m1.cellar prote1.ns.

Table 20. Transition temperatures of Mans Bead and IVS-G

flours, isolates, prote1.nates, micellar proteins

100

and pur1fied prote1ns. 103

Vll

Page 11: Durham E-Theses Aspects of structure and functionality in

List of F1gures

Page Nwnber

F1gure l. Sparg1ng apparatus used for determining foaming

properties. 31

F1gure 2. Relat1onsh1p between cut po1nt and percentage

f1nes of a1r class1f1ed fractions of Marls Bead

and IVS-G flours.

F1gure 3. Relat1onsh1p between cut po1nt and a) percentage

prote1n, and b) percentage starch of au

class1fied fractions of Marls Bead flour.

F1gure 4. Relatlonshlp between cut po1nt and a) percentage

protein, and b) percentage starch of a1r

class1f1ed fract1ons of IVS-G flour.

F1gure 5. Reclass1f1cat1on of the Marls Bead coarse fract1on

obta1ned at 6500 rev./mln.

F1gure 6. Relat1onsh1p between cut po1nt and a) fines y1eld,

and b) f1nes prote1n percentage of sequent1ally

air-class1f1ed fract1ons from Marls Bead and IVS-G

flours.

F 1gure 7. SDS-PAGE of prote1ns extracted from flours,

1solates, prote1nates and m1cellar prote1ns.

F1gure 8. Elut1on profiles of Isolates, proteinates, and

m1cellar prote1ns from Marls Bead after gel

38

42

43

45

49

51

flltratlon chromatography on Superose 6. 52

F1gure 9. Elut1on prof1le of crude globulins from Marls Bead

on HA-Ultrogel. 54

F1gure 10. SDS-PAGE of legum1n and v1c1l1n from Marls Bead

seeds. 55

F1gure 11. Elut1on prof1les of legum1n and v1c1l1n after gel

Vlll

Page 12: Durham E-Theses Aspects of structure and functionality in

filtration chromatography an Superose 6. 57

Figure 12. Analytical scanning ultracentrifugation of llS and

7S proteins from Maris Bead. 58

F1gure 13. Dispersibili ty and gelling characteristics of

defatted Maris Bead proteinate ( 10% solution) • 60

F1gure 14. Dispersibili ty and gelling characteristics of

defatted IVS-G proteinate (10% solution). 61

Figure 15. Dispersibllity and gelling characteristics of

defatted IVS-G proteinate (20% solution). 62

F1gure 16. Dlspersibility and gelling characteristics of

full-fat Maris Bead proteinate (10% solution). 63

Figure 17. Dispersibility and gelling characteristics of

defatted Maris Bead micellar protein (10%

solution). 64

Figure 18. Dispersibil1ty and gelling characteristics of

defatted IVS-G micellar prote1n (10% solution). 65

F1gure 19. Prote1n solub1lity of defatted IVS-G proteinate

( 10% solution) •

F1gure 20. Protein solubility of full-fat Maris Bead

proteinate (10% solution).

Figure 21. Proteln solubility of defatted Maris Bead micellar

protein (10% solut1on).

F1gure 22. Protein solubility of defatted IVS-G micellar

prote1n (10% solution).

F1gure 23. Effect of salt an the dispersibility and gelling

characteristlcs of defatted Maris Bead proteinate

(10% solution at pH 7.7).

F1gure 24. Effect of salt on protein solub1lity of defatted

66

67

68

69

72

Maris Bead proteinate (10% solut1on). 73

F1gure 25. Scann1ng electron m1crographs of gels of Marls

lX

Page 13: Durham E-Theses Aspects of structure and functionality in

Bead isolate, proteinate and micellar protein. 76

F1gure 26. Foam decay curves of selected prote1n standards. 84

F1gure 27. Foam decay curves of pur1fied bean and pea

proteins. 85

F1gure 28. Foam decay curves of soy products. 87

F1gure 29. Foam decay curves of sodium caseinate, spray dried

egg white, and Filby whey protein. 88

Figure 30. Foam decay curves of defatted bean and pea

flours. 89

F1gure 31. Foam decay curves of full-fat bean and pea

flours.

Figure 32. Foam decay curves of defatted bean and pea

Isolates.

F1gure 33. Foam decay curves of

isolates.

F1gure 34. Foam decay curves of

prote1nates.

F1gure 35. Foam decay curves of

proteinates.

full-fat bean and pea

defatted bean and pea

full-fat bean and pea

F1gure 36. Foam decay curves of bean and pea tilicellar

proteins.

F1gure 37. SDS-PAGE of drained liquid from a defatted Marls

Bead isolate.

F1gure 38. DSC theriOOgram of- Maris Bead flour.

F1gure 39. Processing of soy beans.

X

90

91

92

93

94

95

98

102

107

Page 14: Durham E-Theses Aspects of structure and functionality in

rnAPI'ER 1

INTROOOcriCN

The expansion of the food processing industry and the

development of markets for convenience foods have led to greatly

increased demands for low cost protein containing materials. Animal

proteins are expensive in terms of land required for their productlCn,

and market price. Attempts have been made, therefore, to replace them

with alternative sources. Potential candidates have been identified as

oil seed, grain legume, fish, leaf and single cell proteins (Mattil,

1971).

Proteins in foods contribute to both nutritional and

functional properties. In many poorer countries legume proteins are a

maJor source of d1etary protein; in South America 30% of total protein

intake consists· of bean proteins. The use of legumes as protein

supplements 1n low protein cereal based foods ( eg. spaghetti and

bread) has been investigated (Pomeranz and Finney, 1973; Fleming and

Sosulski, 1977; Bahnassey et al., 1986).

However, whilst proteins are nutritionally essential, common

protein foods in developed countries owe their commercial success to

gastronomic appeal. Proteins may contribute specific functional

attributes to foods which give them their characteristic properties,

- 1 -

Page 15: Durham E-Theses Aspects of structure and functionality in

eg. organoleptic, kinesthetic, hydration, surface, structural,

textural and rheological properties. In the food processing industry

the latter properties are more important than nutritional

considerations, since the overall diet is normally balanced for

protein and amino acids anyway. Most attempts to incorporate vegetable

proteins into foods have tried to imitate as closely as possible more

famillar animal protein pro:lucts. This results in a direct campeti tioo

between animal and plant proteins, with the latter required to perform

at least as well as animal proteins before consumer acceptance can be

gained.

Soy proteins are currently the most widely utilized vegetable

proteins In the fabrication of foods. Their physical and chemical

properties have been reviewed by Wolf (1977). However, climatic and

agronomic conditions in temperate regions do not suit the growth

requirements of the soy crop. The E.E.C. must currently import large

quanti ties of soy beans to meet the requirements of the food and

animal feed industries. Econonuc and political reasons make it

desirable to find a substitute crop more suited to the endemic growth

conditions (Hebblethwaite, 1984). One crop under consideration IS

VIcia faba minor. The beans have a relatively high protein content

compared to other grain legumes. Currently V-faba minor seeds are

utilized predominantly in livestock feed compounds, although Interest

in their use in food applications has been expressed, eg. Vaisey et

al. (1975).

Ha.vever, the crop is not very popular in Europe. This has been

attributed to a number of factors (Hebblethwaite, 1984}:

1) low yields in comparison with cereals,

2) low profitability compared to cereals,

- 2-

Page 16: Durham E-Theses Aspects of structure and functionality in

3) unstable yields compared to other crops,

4) uneven maturity in cool temperate countries,

5) disease, eg. Botrytis,

6) problems in utilization and marketing,

7) rapid expansion of more profitable break crops for

cereals, eg. oilseed rape.

rn·contrast to other leguminous crops (eg. soy and Phaseolus

beans) faba bean seeds do not contain harmful concentrations of toxic

constituents. However, they do contain a number of substances which

may Impair nutritional quality, eg. tannins, phytate, protease

Inhibitors, viclne and convic1ne (Nitsan, 1971; Griffiths and Jones,

1977; Martin-Tanguy et al., 1977; Griffiths, 1979; 1981; 1982; 1984;

Moseley and Grifflths, 1979; Fowler, 1980; Griffiths and Thomas, 1981;

Olaboro et al., 1981; Pltz et al., 1981). However, significant

var1ation 1n the content of these anti-nutrit1ve factors In Vlcia faba

lines has been demonstrated, suggesting the possibility of breeding

for varieties with improved nutritlonal qual1ty (Frauen et al., 1984).

In Durham a breeding programme has been undertaken to

construct a faba bean 1deotype based on the 1ndependent vascular

supply reproductive architecture, in an attempt to counter the

unstable yields frequently observed tor this crop (White, 1985). The

most promising seeds produced by this programme were termed 1 IVS-G 1 ,

and their propert1es have been compared with a oommerc1al variety

(Marls Bead) in this study.

- 3 -

Page 17: Durham E-Theses Aspects of structure and functionality in

To facilitate the fabrication of protein foods from cheap raw

materials it is necessary to have an understanding of the structural

and functional properties of the new material. A similar obJective has

already been achieved in the margarine industry, where a fundamental

knowledge of the physical and chemical properties of the relatively

small and less complex glyceride molecules, and the relationship of

these properties to functional and performance characteristics, has

been used to create an acceptable consumer product.

Structural Properties.

The maJor storage proteins of VIcia faba are globulins, and

can be separated into two maJor types termed legumin and vicilln. The

widespread occurrence of homologous proteins has been demonstrated in

many dicotyledonous plants, and also in some monoootyledenous ones

(Derbyshire et al., 1976). They are characterised by their complex

quaternary structure, a tendency to association - dissociation

reactions, low contents of a-helix (approx. 10%), and a large {3-sheet

complement (approx. 50%) (Fukushima, 1968; Blagrove et al., 1984;

Zirwer et al., 1985).

Legumin from V. faba has been studied by Bailey and Boulter

(1970), Wright and Boulter (1974), Mori and Utsumi (1979), Utsumi et

al. ( 1980) and Matta et al. ( 198la), and has been compared to pea

legumin by Croy et al. ( 1979). The accepted model of legumin structure

IS a protein with an approximate Mr. of 340 000, comp::>Sed of SIX

acidic + basic subunit pairs. This has been supfXJrted by small-angle

x-ray scattering (SAXS) studies of V.faba legumin in solution (Plietz

et al., 1984). Sulilar structures have been observed for pea legumin

(Miles et al., 1985), soy glycinin (Badley et al., 1975; Miles et al.,

1984), and the 115 proteins from sunflower and rape seeds (Plletz et

- 4 -

Page 18: Durham E-Theses Aspects of structure and functionality in

al., 1978; 1983b).

The legumin subunits from V. faba exhibit a considerable degree

of heterogeneity (Wright and Boulter, 1974; Utsumi and Mori, 1980;.

Matta et al., 198la; Maplestone et al., 1985). Similar heterogeneity

has been observed for US proteins from pea (Thomson et al., 1978;

Thomson and Schroeder, 1978; Krishna et al., 1979; Matta et al.,

198lb), soy bean (Kitamura et al., 1980; Mon et al., 198lb), ground

nut (Tombs, 1965) and lupin (Blagrove and Gillespie, 1978).

Each acidic + basic subunit pair is JOined by a disulphlde

linkage, and pairing between subunits IS specific (Staswick et al.,

1981; Matta et al., 198lb; Utsumi and Mori, 1983; Horstmann, 1983).

· Thls is due to the synthesis of the subunit pairs as single

polypeptides and subsequent processing by proteolytic cleavage of the

precursors. Precursors have been identified in pea (Evans et al.,

1979; Croy et al., 1980; 1982; Lycett et al., 1984; Boulter, 1984),

V.faba (Croy et al., 1980), soy (Turner et al., 1981; 1982; Barton et

al., 1982; Nielsen, 1984}, rice (Yamagata et al., 1982) and oats

(Brinegar and Peterson, 1982; Matlashewski et al., 1982; Walburg and

Larkins, 1983).

Vicilin from VIcia faba has been studied by Bailey and Boulter

(1972) and Mori and Utsumi (1979). Native vicilin exists as a trimer

with an approximate Mr. value of 120 000. The shapes of 7S proteins In

solution have been observed using SAXS for phaseolus beans (Plietz et

al., 1983a; c), and pea (Miles et al., 1985}. Three 'Y' shaped

subunits with deep solvent clefts have been observed. Association is

controlled via hydrophobic interactions. Considerable heterogeneity of

vicilin proteins has also been demonstrated.

- 5 -

Page 19: Durham E-Theses Aspects of structure and functionality in

The maJor differences between the legumin and vicilin proteins

are:

a} the larger size of the legumin protein,

b) the Involvement of disulphide linkages in stabilizing the

subunit structure of legumin,

c) the higher sulphur containing amino acid content of legumin,

d) the small quantities of carbohydrate associated with vicilin

(Gatehouse et al., 1980: 1981}.

However, structural similarities between legumin and vicilin

storage proteins have been demonstrated (Argos et al., 1985).

Legumins from different· legumes also show significant

homology. Wnght ( 1983} ccmpared the amino acid content of pea, field

bean and soy bean legumins. Only proline, arginine and threonine

contents differed by more than 10%, and these differences were less

than 20%. Pea and field bean legumins were more closely related than

either of these two with soy beans. Generally non-_polar and

dicarboxylic acid residues were conserved.

Amino acid sequence homology between subunits, and. between

legume proteins from different species, has been demonstrated by

Gilroy et al. (1979}, Moreira et al. (1979}, Casey et al. (l98la: b)

and Walburg and Larkins ( 1983} •

Soy protein structure has been reviewed by Badley et al.

(1975) and Peng et al. (1984).

- 6 -

Page 20: Durham E-Theses Aspects of structure and functionality in

Cons1dering the extent of the similarities between storage

proteins from a variety of plant sources it would seem reasonable to

expect similar functional properties. However, large quant1ties of

purif1ed proteins are not easily obtainable without considerable

effort and expense, and this renders them impractical for use by the

food industry. However, a variety of processing methods have been

developed to produce useful materials for food fabrication. These

materials range widely in their physical, chem1cal and functional

properties, and can be tailored to meet the requuernents of spec1fic

products. The processing methods used in this thesis were defatting,

a1r class1fication, and isolate, prote1nate and m1cellar protein

preparation.

Air classiflcation 1s a technique in wh1ch part1cles differ1ng

1n s1ze, density and mass are separated 1n a current of air. By

careful select1on of the operating cond1tions it is possible to

determ1ne the compos1t1on of the coarse and fines fract1ons produced.

The technique has proved useful for producing protein rich and starch

rich fract1ons 1n1tially from cereals, and subsequently from many

starchy gra1n legumes, eg. california small white beans ( Kon et al. ,

1977), navy beans (Patel et al., 1980) field peas and horse beans

(Vose et al., 1976), mung beans and lentils (Sosulski and Youngs,

1979; Tyler et al., 1981}. Its application to wheat, barley, malted

barley, oats, triticale, rice, sorghum, potatoes and gra1n legumes has

been reviewed by Vose {1978}.

The procedure for isolate product1on was first developed for

soy beans (Anson and Pader, 1957}, but has been adapted for rape seed

(Glllberg and Tornell, 1976), faba beans (Bramsnaes and Olsen, 1979),

mung beans {Thompson, 1977), phaseolus beans (Satterlee et al., 1975),

lup1ns (King et al., 1985}, peas and horse beans (Vose, 1980) and

- 7 -

Page 21: Durham E-Theses Aspects of structure and functionality in

cotton seed (Lawhon and cater, 1971). Commercial producticn of

isolates usually involves alkaline extraction of proteins from the

flour and removal of insoluble material, followed by precipitation of

the protein at the isoelectric point. The isolate is then washed and

spray dried, or neutralized with sodium hydroxide and spray dried as a

sodium proteinate. The ultimate aim of the method is to ootain an

efficient protein extraction, and to rec6ver the protein in a soluble

form so that its functional properties can be fully exploited. The

method of protein isolation may influence the functional properties of

a protein to a greater extent than the actual nature of the protein.

Therefore, it IS important to avoid harsh extraction or precipitation

conditions. Large yields of isolates can be obtained from food sources

possessing proteins with good solubility characteristics at the

extraction pH, and low solubility at the isoelectric point.

An even gentler processing method IS used in the production of

micellar proteins. The procedure was developed using field beans and

exploits hydrophobic interactions between protein molecules (Murray et

al., 1978). Many food proteins have high hydrophobicity values and a

tendency to form quaternary structures (Bigelow, 1967). Same of these

hydrophobic residues may be exposed on the surface if insufficient

polar residues are available to bury them in the interior of the

IIOlecule (Klotz, 1970; Lee and Richards, 1971) and these would tend to

come together in an aqueous environment if they were present in

sufficient concentrations. To enhance this reaction pH should be close

to neutrality as at more extreme pH values repulsion between charged

am1no acid residues will result in increased solubility. When these

hydrophobic reactions occur extensive protein precipitation takes

place, and the micellar protein can be collected and dried. Once

formed the protein micelles are relatively stable, possibly due to the

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formation of d1sulphide linkages. The effects of Iii and various an1ons

on micellar protein formation b¥ vicilin from V1cia faba have been

1nvest1gated by IsiOC>Ild et al. (l986a: b).

Generally protein is extracted 1n a weak salt solution. The

supernatant is then diluted w1th distilled water to promote

hydrophobic 1nteractions (Murray et al., 1981). Micellar proteins can

be produced by th1s method from field peas, chickpeas, peanuts, rape

seed, soy beans and oats (Murray et al., 1981). Other proteins which

have the capacity to aggregate 1nto a ml.cellar arrangement include

~-casein (Evans and Phillips, 1979) and membrane proteins (Slmons et

al., 1978). Electrolyte med1ation 1s essential for the format1on of

case1n m1celles (Slattery, 1976).

The mer1ts and problems associated w1th these methods are

d1scussed at greater length 1n the discussion.

Functional Properties~

To assess the funct1onal properties of new proteins a

systemat1c evaluation of the1r behav1our in a var1ety of env1ronments

has to be undertaken (Kinsella, 1976: 1979). Traditionally new

1ngredients were tested in food products under pract1cal cond1t1ons.

This approach is expensive and time consuming, although ultlmately 1t

1s necessary before a new food prote1n is accepted in a marketable

product. Many s1mple model functional tests have been developed with

the 1ntent1on of measur1ng the behav1our of proteins obJectively and

of extrapolating the results to predict behav1our in food systems.

Ideally tests should be performed us1ng a w1de range of pH values,

salt concentrat1ons, temperatures and 1n the presence of various 1ons,

to represent the range of conch tions found 1n food systems. The

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development of m1cro-methods which are qu1ck, accurate and use small

quant1t1es of material facilitates this process. Micro-methods have

been developed to assess foam1ng {Wan1ska and Klnsella, 1979; Kato et

al., 1983b), gell1ng {Utsumi et al., 1982) and emulsifying {Yamauch1

et al., 1982) properties. Hawever, these methods are not in widespread

use.

a) Solubility.

Many important functional properties of food proteins relate

to water-protein interactions, eg. solubility and dispersibility,

v1scos1ty, gelation, foaming and emulsification (Kinsella, 1976;

Hermansson, 1979). A solubillty profile of a new food protein will

provide information important for determ1ning a) the optimum

extraction procedure for that protein, and b) 1ts potent1al

appllcation in fabricated food systems, eg. maximum solubility at

acidic pH values for carbonated beverages, or good solubility and an

absence of heat prec1pitation 1f the protein is to be used in m1lk

type beverages or coffee whiteners {Wolf and Cowan, 1971). The balance

between protein-protein and protein-solvent interactions can be

affected by pH, concentrat1on, temperature, nature of the solvent,

processing method and presence of other components, eg. llpid and

phytate (Hermansson, 1979; de Rham and Jost, 1979).

For maximum functionality, solubility should be high over a

broad pH range; low solubllity over a broad pH range 1s generally a

sign of severe denaturation. Wolf and cowan (1971) suggested that the

nitrogen solub1lity index (NSI) proVldes useful informatlon concem1ng

the extent of heat damage sustained dur1ng the pcocessing of soy

beans. The effects of processing methods on subsequent solubility have

been studied for 1solates from soy bean and rape seed (Hermansson,

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1979), coconut (Samson et al., 1971), peanut (Rhee et al., 1973),

alfalfa leaves (Lu and Kinsella, 1972) and cottonseed (Lawhon and

cater, 1971). However, a better methcxl of determining the extent of

protein denaturation is differential scanning calorimetry (OOC). This

1s a useful thermoanalytical technique for monitoring changes 1n

phys1cal or chemical properties of materials as a function of

temperature. Its use in food research has been reviewed by Biliaderis

(1983). An inert material and a sample are heated at a constant rate,

and the differential heat flow to the sample is recorded as a peale

The area under the peak is directly proportional to the enthalpic

change in the sample. A relat1vely undenatured protein would be

expected to produce a larger enthalpic change than a denatured one. In

this study the effects of the processing method used on the

d1spers1bility prof1les and DSC thermograms of protein products were

investigated.

b) Gelling.

Heating an aqueous prote1n d1spers1on often causes an increase

1n viscos1ty, and at suffic1ently h1gh concentrations gelling may

occur. This property is important in foods where thickening or gelling

properties are required, eg. custard type puddings, sauces, soups,

beverages, batters, sausage type meats, cheese, yoghurt and baked

products. Egg and muscle proteins, wheat gluten and carbohydrates have

been traditionally employed as thickening or gelling agents. Heat1ng

an 8% solut1on of soy prote1n may cause gelation ( catsimp:XJlas and

Meyer, 1970). However, gels from globular proteins generally require

10 x the protein concentrat1on compared to gels formed from gelat1n or

carbohydrate sources (Tombs, 1974).

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Gels can be described as a 3-dimensional network structure

wh1ch may act as a matrix to hold water, lipids, dissolved proteins,

carbohydrates and other food components. Muscle proteins are largely

responsible for the physical and chemical stabilization of fat and

water in conuninuted meat prc:xiucts (Ziegler and Acton, 1984: SameJlma

et al., 1985; Hermansson et al., 1986). The mechanisms involved in gel

formation are difficult to study as most current rheological

instruments are des1gned to evaluate the final prc:xiuct. However, the

gelat1on mechanisms of egg proteins have been studied by Hegg et al.

(1979), Nakamura et al. (1982), Gossett et al. (1984), Grinberg et al.

(1985) and Watanabe et al. (1985). Many studies have also been made on

the gelling mechanisms of soy proteins and these are more extens1vely

rev1ewed in the d1scussion.

c) Foaming.

The behaviour of proteins at Interfaces is of fundamental

s1gnificance 1n toad systems such as emulsions and foams. Foams are

found in whipped toppings and creams, souffles, mousses, meringues,

ice cream, leavened bread and baked prc:xiucts. They are enjoyed for

the1r lightness and mouth feel. Foam formation involves the entrapment

of a1r by a protein film, and these air cells act to impart bc:xiy and

smoothness, ensure uniform rheological properties and facilitate

d1spersion of flavours in the prc:xiuct. Egg white 1s currently the most

widely used foaming agent, but gelatin, casein, milk, whey prote1ns,

gluten and soy prote1ns are also used (Kinsella, 1981).

There are three widely used methods for determimng foam1ng

properties: a) whipping {Eldridge et al. I 1963; Lawhon and cater I

1971), b) shaking (Yasumatsu et al., 1972; Wang and Kinsella,. 1976)

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and c) sparging (Buckingham, 1970; Mita et al., 1977). The anount of

protein usually employed in each test varies, ie. 3-4% for whipping,

1% for shaking and 0.1-2% for sparging. The volumes required are also

much larger for whipping. Proteins are subjected to different forces

during foam· formation by the three methcx:is. Foam bubbles are

continuously formed and broken by shear forces during whipping. In

contrast, once bubbles are formed by sparging the rate of rupture IS a

function of lamella thickness and interfacial viscoelasticity (Mita et

al. , 1977) • The methcx:is of prcx:iucing foams have been compared by

Halling (1981). In this study results obtained by the sparging and

whipping methoos were compared.

d) Emulsifying properties.

Emulsifying agents are used extensively in focx:is such as

coffee whiteners, milk type beverages, mayonnaise, gravies, comminuted

meats and ice cream. The most widely used emulsifying Ingredients are

meat and milk proteins.

Three indices of emulsifying properties are in general use,

(1} emulsifying capacity ( EC ), (2) emulsion activity ( EA) and

{3) emulsion stability ( ES ) • The EC index was introouced by Swift et

al. {1961}. A protein solution is vigorously stirred while oil is

steadily added. When a critical volume of added oil is reached the

solution undergoes a sudden change in viscosity, and this is taken as

the end point of the titration. Using EA as an index was introouced by

Yasumatsu et al. (1972). An emulsion is formed by mixing set volumes

of oil and protein solution. This is then centrifuged and the height

of the unseparated layer IS measured. Determining ES involves

monitoring the rate of depletion of oil from the bottom of an emulsion

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over a time period.

The effects of different blending methods, and speed and

durat1on of blending on emulsion formation have been 1nvestigated by

Tornberg and Hermansson (1977} and Pearce and Kinsella (1978}.

Generally increasing blending speed results in smaller oil droplets

and a decreased % oil phase volume (Swift et al., 1961; Carpenter and

Saffle, 1964; Ivey et al., 1970; Crenwelge et al., 1974}. The type of

011, protein concentration and oil volume fraction also affect

emuls1on tormat1on (carpenter and Saffle, 1964; Pearce and K1nsella,

1978}. This makes 1t difficult to compare results obtamed by

d1fferent groups. comparat1ve stud1es of emuls1fying properties of

vegetable prote1ns have been made for chick pea, faba bean, field pea,

great northern bean, lentll, lima bean, lupin, mung bean, pea bean,

peanut, pecan, rape seed, soy bean and sunflower proteins ( Inklaar and

Fortuin, 1969; Lin et al., 1974; Sosulski et al., 1976a; Hutton and

Campbell, 1977; McWatters and Cherry, 1977; Ramanatham et al., 1978;

McWatters and Holmes, 1979a; b; Volkert and Kle1n, 1979}. A review on

the use of vegetable proteins as emulsify1ng agents was conducted by

McWatters and Cherry (1981}.

Alms.

The aims of this study were to compare the structural and

funct1onal propert1es of protein-based products prepared from a

commerc1al bean variety (Maris Bead}, w1th those from the new IVS-G

line. Also, a var1ety of processing methods were used to produce

mater1als with a range of phys1cal and chemical propert1es, and these

were assessed for functionallty in a number of simple tests. The

potentlal of a dry processing method, namely au classificat10n, for

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producing protein concentrates w1th equ1valent protein contents and I

functional properties to commercial soy products was assessed. The

functional properties considered were solubility, dispersibility,

gelling, thermal, foaming and emuls1fying. Any observed functional

differences should reflect the variations generated by the processing

methods 1n chemical and phys1cal properties, and lead to a better

understanding of the relat1onships between these properties and

functional properties.

The ultimate a1m was to assess, in terms of functionality, the

potential of the field bean preparations as competitors to those of

the soy bean as a source of protein for the food industry.

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2 .1 BIOI.miCAL MATERIALS.

CEAPI'ER 2

MATERIALS

Seeds of Vicia faba minor cv. 'Maris Bead' were obtained from

Tynes1de Seed Stores, Gateshead, Tyne and Wear. Seeds of V1cia faba

(IVS-G) were donated by Dr. P. Gates, Department of Botany, Umvers1ty

of Durham.

Scd1um case1nate was obta1ned from Unilever Research, Colworth

Lab::>ratory, Sharnbrook, Bedfordshire, MK44 li.Q.

Full-fat and defatted soy meal were obtained from British Drug

Houses (BDH) Limited, Poole, Dorset, BH12 4NN.

Soy protein concentrate was supplied by Lucas Ingredients

Lim1ted, Morav1an Road, Kingswocd, Bristol, BSlS 2NG.

Pea (B1rte, F1lby or Progreta) and soy concentrates, isolates,

prote1nates and micellar proteins were prepared at the AFRC Institute

of Focd Research, Norwich Lab::>ratory, Colney Lane, Norwich, Norfolk,

NR4 7UA.

Pea (Birte) globulins, and 7S and llS fract1ons were also

produced at the AFRC Institute of Focd Research. The globullns were

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obtained by salt extraction, and the 7S and llS fractions by ammonium

sulphate precipitation.

Spray dried egg white was supplied by Allmey and Layfield

Limited, Windsor Mills, Holden Street, LiverpJOl.

Purified proteins were obtained from the Sigma Chemical

Compcmy, Fancy Road, Poole, Dorset, BH17 7NH. They were: BSA type

A4503, ~-globulin type G5009, hemoglobin type H2500, lysozyme type

L-6876, myoglobin type Ml882 and ovalbumin type 5503.

2. 2 CHEMICALS AND REAGENTS.

Trizma base and coomassie brilliant blue R were obtained from

the Sigma Chemicals Company, Fancy Road, Poole, Dorset, BH17 7NH.

All other chemicals were supplied by British Drug Houses

(B.O.H.) Ltd., Poole, Dorset, BH12 4NN, and were of AnalaR grade or

the best available.

2. 3 arHER MATERIALS.

HA-Ultrogel was obtained from LKB Instruments Ltd., South

Croydon, Surrey, CR2 840. Superose 6 was obtained trom Pharmacia

(G.B.) Ltd., London, WS SSS.

Visking dialysis tubing was supplied by Medicell International

Limited, 239, Liverpool Road, London, Nl.

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QIAPI'ER 3

MEI'IDDS

3.1 PREPARATICN OF EXPERIMENTAL MATERIAL.

3.1.1 Preparation Of Flour For ~r-classificatlon.

Seeds were spl1t on a Pascal End Runner Mlll and the spl1ts

passed through an Alpine Kolloplex 160Z p1n mill, as descr1bed by

Wr1ght et al. (1984).

3.-1.2 Preparat1on Ot Flour For Protein Pur1flcat1on.

Seeds were dehulled manually and freeze--dr1ed. The cotyledons

were ground for 30 s 1n a water-cooled Janke and Kunkel mill. The

flour was defatted tw1ce with hexane (1:10 w/v) at 4°C for 30 m1n.

Excess hexane was removed under vaccuum.

3. 2 FRACI'IONATICN OF FLOURS.

3.2.1 A1r-class1ficat1on.

Flour was fractionated using an Alpine Zig-Zag Class1f1er

model AlOO MZR. Class1flcat1on of flours was mvest1gated using

class1fier speeds

oorrespond1ng a1r

rang1ng

flows

from 3000 to 11000 rev./min, and

from 52 to 44 N m3h- 1 • Percentage we1ght of

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coarse and f~nes fract~ons was determined for each experiment. Due to

unavoidable losses from the fines fraction, percentage weight of fines

was calculated as 100 - percentage we~ght of coarse fract~on. All

we~ghts were corrected for moisture content to negate the effects of

water loss dur~ng the air-classification process.

3.2.2 Re-class~f~cation Of Coarse Fraction.

1 kg Mar~s Bead flour was air-classif~ed at 6500 rev./rnin.

Th~s speed was chosen as ~t produced the coarse fraction w~th the

h~ghest protein content when both prote~n percentage and fract~on

y~eld were cons~dered. The coarse fract~on was re-milled as descr~bed

prev~ously. 200g twice-milled flour was re-classif~ed at 5500, 6500

and 7000 rev./rnin. The percentage we1ght of the coarse and fines

fractions was determ~ned.

3.2.3 Sequential Air-class1f1cat1on.

lkg Maris Bead and IVS-G tlours were milled as described

prev~ously. 600g flour was a1r-class~fied at 11000 rev./min. The

coarse fract~on was re-class~fied at 9000 rev./min, and the process

repeated at 8000, 7000, 6500, 6000, 5500, 5000, 4000, and 3000

rev./mln. Percentage weight of coarse and fines fractions was

determ~ned after each air-class~f~cat1on.

3.2.4 Protein Yield, Prote~n Separat~on Efficiency, Starch Y1eld And

Starch Separation Efficiency.

Prote1n Yield (P.Y.) and Prote~n Separat~on Efficiency

(P.S.E.) were calculated as defined by Tyler et al. (1981).

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P.Y. = weight fines x + % weight coarse x protein in fines % protein in coarse

% protein In starting material

P.S.E. = 100 - (% weight coarse x % protein in coarse) % protein in starting material

Starch Yield (S.Y.) was determined by the same method as

(P.Y.). Starch Separation Efficiency (S.S.E.) was obtained from the

following equation:

S.S.E. = 100 - (% we1ght fines x % starch in f1nes) % starch 1n starting material

3. 3 ANALYSIS OF FI.CX.JRS AND AIR-cr.ASSIFIED FRACI'ICNS.

3.3.1 Moisture Content Determination.

0 Moisture content was measured by dry weighing samples at 105 C

overnight. Tests were performed In duplicate.

3.3.2 Protein Determination.

Nitrogen content of oven-dried samples was measured using a

Carlo Erba N!lA. 1400 Automatic Nitrogen Analyser (N x 6.25). All

results were the average of duplicate tests. A nitrogen to protein

conversion factor of 6.25 was used throughout this thesis for ease of

comparison w1th other funct1onal1ty studies.

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3.3.3 Starch Determination.

Starch determination was conducted on oven-dried samples

according to the glucoamylase methcxi of Blake and Coveney ( 1978). All

results were the average of duplicate tests.

3. 4 ISOIATE, PROI'EINATE AND MICELLAR PROI'EIN PROcucrioo.

Isolates and proteinates were produced by a modification of

the method of Sumner et al. {1981).

3.4.1 Isolate Preparation.

Flour was extracted In water (1:10 w/v) at fH 7 and rCXJIII

temperature for 1 h, centrifuged and the supernatant fract1.on

collected. The pH of the supernatant fraction was adJusted to 4.6

4.7 and the precipitate centrifuged and collected. It was resuspended

In a small quantity of distilled water and freeze dried.

3.4.2 Proteinate Preparation.

The isolate procedure was followed as far as the second

centrifugation. The precipitate was resuspended In a small quantity of

distilled water and the pH adJusted to > 7. It was stirred unti1

stable and freeze dried.

3.4.3 Micellar Protein Preparation.

(a)

Flour was extracted In 0.4M NaC1 (1:10 w/v) at fH 6 and

room temperature for 30 min. The mixture was filtered

through two layers of muslin and the filtrate centr1fuged.

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(b)

The supernatant was reduced 1n volume by 80% using an

Am1con Model DC2 laboratory dialyzer/concentrator and

d1luted (1:5} with chilled, distilled water. The

precipitate was allowed to settle. The supernatant was

decanted and the residue centr1fuged and freeze drled.

Micellar protein was prepared by a modif1cation of the

method of Murray et al. (1978}. Flour was extracted in

0.4M NaCl (1:10 w/v} at pH 7 and rOCl!II temperature for 3 h.

The mixture was centrifuged. The supernatant fract1on was

d1luted (1:3} Wlth ch1lled, d1st1lled water and left at

4°C overn1ght. The precip1tated protein was collected

(after an extra centr1fugat1on 1f necessary) and freeze

drled.

3. 5 f'URIFICATION OF SI'ORAGE PROI'EINS.

Extraction and pur1fication of the 78 and llS storage prote1ns

was conducted by a modif1cat1on of the method of Gatehouse et al.

(1980).

3.5.1 Crude Extract1on Of Storage Proteins.

Defatted flour was extracted (1:10 w/v) m 50nM potasswm

phosphate buffer w1th 0.4M NaCl, pH 7.8 at 4°C for at least 3 h. The

m1xture was centrifuged at 20000 g for 30 min and the pellet

d1scarded. The solut1on was fractionated by {NH ) SO prec1p1tat1on, 4 2 4

and the material prec1pitat1ng 1n the range 60 - 100% saturatlon was

collected by centr1fug1ng at 20000 g for 30 min. The crude globul1n

pellet was resuspended 1n 50rrM potasswm phosphate (pH 7 .8} and

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d1alyzed extensively into the same buffer.

3.5.2 Separation Of Crude Globulins On HA-Ultrogel.

Buffers contained 0.05% (w/v) sodium azide and were filtered

through 0.22 f.LM pore size cellulose acetate filters. The dialyzed

globul1ns were filtered as above and loaded on to a column of

HA-Ultrogel. Excess extract was eluted by washing with 50mM potassium

phosphate buffer, pH 7. 8. The column was eluted with a linear

concentrat1on gradient of potassium phosphate buffer, pH 7. 8 ( 50mM -

0.75M, 500 ml + 500 ml), at a flaw rate of 40 ml/h. 10 ml fractions

were collected and freeze dned. They were subsequently analyzed by

SDS-PAGE.

3.6 ANALYSIS OF PROTEINS.

3.6.1 Polyacrylamide Gel Electrophoresis (PAGE).

(a) Preparation of samples for SDS-PAGE.

The follaw1ng procedure was used for samples already in

solut1on. 200 ~1 sample containing approximately lOO~g

protein was taken and 1.2 ml 0.05% 880 NH3

m acetone

added. The solution was chilled at -20°C for 20 run. The

sample was centrifuged at roam temperature and the

supernatant decanted. Excess acetone was allowed to

evaporate. 95 ~ lOrrM Tris, 5mM EIJI'A, 20% (w/v) SDS

(pH 7 .85) and 5 ~1 2-mercaptoethanol were added. The

sample was mixed thoroughly.

(b) SOO-PAGE.

Samples were run on 15% (w/v) fOlyacrylamide slab gels

accord1ng to the system of Laermnli ( 1970). Molecular

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weights were determined using the following standards:

phosphorylase b (Mr. 92000), BSA (67000), ovalbumin

( 45000) , lactic dehydrogenase ( 35000) , chymotrypsinogen

(25000), ~-lactoglobulin (18500) and ribonuclease (12500).

3.6.2 Analysis Of Purified Proteins On Superose 6.

To test homogeneity the purified proteins were passed through

a Superose 6 gel filtration column according to the method of Lambert

( 1985). All buffers contained 0.02% (w/v) sodium azide and were

filtered through 0.22 ~m cellulose acetate membrane filters. The

samples were dialyzed in 50rnM Tris, 200rnM NaCl, lmM IJIT (fii 8.0), at

4°C overnight. They were filtered and loaded on a 10 ml Superose 6

column and eluted at a flow rate of 0.4 ml/ffiln. Retention times were

compared to the following standards: thyrogldbin (Mr. 669000),

ferritin ( 440000), glucose oxidase ( 154000), BSA ( 67000), ovalbumin

(45000) and myoglobin (18000).

3.6.3 Analytical Ultracentrifugation.

Samples were tested for homogeneity on an MSE Centriscan 7S.

0.5-5% (w/v) protein solutions were dialyzed Into 0.035M KH2P0

4 , 0.4M

NaCl, lmM OTT, 0.05% (w/v) sodium azide (pH 7.6), at 4°C for 16 h.

Samples were centrifuged at 50000 rev./min and 20°C. Scans were made

at 10 min intervals and sedimentation coefficients were measured and

corrected to S20

,w values using density and viscosity values given by

Svedberg and Pederson ( 1940) • Values of S , w were obtained at four 20

protein concentrations and 0

S20

,w values calculated by linear

regression analysis.

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3. 7 MEASUREMENT OF SOLUBILITY AND GELLING ABILITY.

3.7.1 Measurement Of SolUbility And Gelling Ability As A Function Of

InsolUble aggregates, solUble aggregates, nitrogen solubility

and gelling ability were measured for solutions of proteinates,

Isolates and micellar proteins over the pH range 2 - 11.

Samples were homogenized in distilled water (10 or 20% w/v)

until a homogeneous dispersion was obtained. 18 ml aliquots were

adJUSted to the desired pH level with dilute acid or alkali. 2 x 8 ml

were transferred to a graduated centrifuge tUbe {10 ml) and

centrifuged In a MSE Minor (Setting 5) for 5 min.

(a) Measurement of insoluble aggregates.

InsolUble aggregates were measured as the volume of

precipitate (cm 3) after centr1fugat1on.

(b) Measurement of soluble aggregates.

Soluble aggregates were measured by reading the optical

density at 420 nm after centrifugation, using distilled

water as the zero value.

(c) Measurement of soluble protein.

SolUble protein was determined by the method of Lowry et

al. (1951), with BSA as the standard. 500 ~1 aliquots were

taken from each sample before gelllng. DupliCates were

taken at two concentrations for each sample.

(d) Measurement of gelling ability.

()

Samples were gelled in the centrifuge tUbe at 95 C for 30

min. They were allowed to cool and left at 4°C overnight.

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Samples were centrifuged in a MSE Minor (Setting 5) for 5

m1n and the volumes of gel and supernatant recorded. A

qual1tative assessment of the gel was conducted (Voutsinas

et al., 1983b). Gels were ass1gned a number on the

following scale:

-4: a smooth liquid

-3: a sl1ghtly granular liquid

-2: a moderately granular l1qu1d

-1: granular but collapses w1th inversion

0: a viscous gel-like semi l1quid

+1: a soft gel

+2: a medium gel

+3: a fum gel

3.7.2 Assessment Of Gell1ng Propert1es By A Compression Test And

Stress Relaxat1on Measurements.

Compression and stress relaxat1on measurements were performed

us1ng an Instron Un1versal Test1ng Machine, Model 1122. Samples were

homogenized 1n d1stilled water (1:10 w/v) until a homcgeneous

d1spers1on was obtained. The pH was adJusted and the sample

centrifuged 1n a MSE M1nor (Setting 5) for 10 min. The solution was

poured 1nto the templates ( 15rrun diameter teflon cylinders embedded in

a steel block) and gelled at 95°C for 30 min. The gels were allowed to

cool and left at 4 °C overnight. Gels were removed from the templates

and coated with s1licon fluid (Dow corn1ng 200/100 cs) to prevent

evaporat1on. Pr1or to test1ng the crosshead platen and steel plate

were also coated.

- 26 -

Page 40: Durham E-Theses Aspects of structure and functionality in

(a) Compression test.

The sample was compressed at 50mm/min until material was

expelled from between the platens. The stress induced in

the sample was measured against time and data recorded

us1ng a Hewlett Packard HP85. Data was fitted to the

following expression (Blatz et al., 1974).

F~ = 2 G (An -A-m) n

Where F~ = stress

= new he1ght initial height

G = shear modulus or 'r1gidity'

n = a material constant

Rupture strength (Nm- 2) was expressed as the force applied to

the sample when the surface yield point was reached.

(b) Stress relaxat1on measurement.

The sample was compressed at a constant rate (50 nun/m1n)

to a pre-determined strain. The stress detected by the

load cell was recorded using a Hewlett Packard HP85. Data

collect1on was stopped when no signif1cant change in

signal was observed. Relaxat1on t1mes were abta1ned by

curve f1tt1ng the data to an exponential ser1es (Peleg and

Normand, 1983) of the form:

Where F00 is the residual force at '1nfinite' t1me

A = the ampl1tude of the 1ndiv1dual stress components

T = time requued for a stress camp:x1ent to reduce by 1/e

F(t) = the decaying parameter (1e. force)

- 27 -

Page 41: Durham E-Theses Aspects of structure and functionality in

Force ~s used here as the area is assumed to be constant

throughout relaxation.

Co-operat~ve flo.v analysis as described by Bohlln (1980) was

carried out on the data using the calculated relaxation times. The

theory considers viscous flow to be the major component in stress

relaxation, and that a flow un~t can be ~dentifled. The relationship

between a flow unit and the bulk system is defined by the cooperat~ve

coord~nat~on number, -z . The rate equat~on describ~ng the relaxation

process ~s given by:

ds = -( 1) s(s+~)z dt -7- -

where s = relat~ve stress (or force)

7 = the relaxation time

a = a measure of the strength of the cooperativity

The co-ord~nation number, z, was obta~ned duectly fran the inverse

slope of the linear section of a graph of

-d (F/~) d lnt

versus

where F = force

F~ = the ~n~t~al force

t = time

The intercept of this l~ne with the F/~ ax~s was also

recorded.

3. 8 ASSESSMENI' OF FOAMING ABILITY.

3.8.1 Determination Of Foam~ng Ab~l~ty By A Large-scale Wh~pp~ng

Method.

Foam~ng abil~ty was determ~ned by a rnod~f~cat1on of the method

- 28 -

Page 42: Durham E-Theses Aspects of structure and functionality in

of Patel (1985). 250 ml 0.5% (w/v) solution in O.lM potass1um

phosphate (pH 7), was stirred for 1 h at room temperature. The

solut1on was transferred to a Kenwood Chef Model A901 with a balloon

whisk attaclunent and whipped at maximum speed for 5 min. The foam and

res1dual l1quid were transferred to a 2 1 measuring cyl1nder with a

plastic spatula. Air pockets in the foam were removed by two sharp

downward shakes. 3 .

The total volume (em ) and volume of drained llqu1d

(em 3

) were measured and recorded 5 min after whipping had flmshed

(To), and at 10 min 1ntervals for 1 h. Dupl1cates were performed for

each sample. The results were used to calculate ·the following

parameters:

(a) Foam Expansion (F.E.)

F.E. = (1nit1al foam volume (cm 3) - 250) x 100

250

where 1n1tial foam volume includes the residual l1quid

volume.

(b) Foam Volume Stabllity (F.V.S.)

F.V.S. = foam volume (cm 3) after 30 minx 100

initlal volume of foam (cm 3 )

where in1tial foam volume 1ncludes the residual l1qu1d

volume.

(c) Foam Liquid Stabllity (F.L.S.)

% Llquid Drainage (L.D.)

F.L.S.

= Volume of liqu1d drained (cm 3}

after 30 min 250

= 100 - L.D.

- 29 -

Page 43: Durham E-Theses Aspects of structure and functionality in

3.8.2 Determ~nat~an Of Foam~ng Ab~l~ty By A Small-scale Sparg~ng

Method.

Foaming ab~lity was measured by a modification of the method

of Kato et al. ( 1983b}. The apparatus is sham in Figure 1. The flow

rate was set at 50 cm3 min· 1 using 5cm 3 distilled water. The sinter and

burette were cleaned and dried. 25 ml of 0.5% (w/v} solution ~n O.lM

potassium phosphate buffer (.pH 7} was stured for 1 h. 5 ml was

pipetted ~nto the burette. Gas was duected through the vent unt~l the

flow rate was stable and then reduected through the sinter for 1 min.

Data was recorded on a chart recorder for 10 min after sparg~ng.

Readings were taken manually from the chart recorder at 0. 25 m~n

intervals and a !~near regression obtained for the time interval l - 4

min. Each sample was tested in dupl~cate. It was essential to use the

same s~nter throughout the experiment and to clean it w1th chr~c

acid between samples to obtain reproducible results.

Foam expansion and foam stability were determined by two

methods, as descr1bed by Kato et al. (l983b}.

F~rstly, foam expansion was determined by measur1ng the

canduct~v~ty of the foam immed1ately after sparging was complete, i.e.

~n~t1al canduct~vity (Ci}. Foam stabil1ty was obta1ned from the

follow~ng equat~an:

Where

eo.f:..t/&

f:..t is represented by the t1me interval 1 - 4 m~n.

f:..c ~s the change in conduct1v1ty, c, occurnng dur1ng

the t1me 1nterval f:..t.

and Co 1s the conduct1v1ty at 0 t1me obtained from the

extrapolatlon of a linear conduct1vity versus time

plot for the t1me 1nterval 1 - 4 m1n.

- 30 -

Page 44: Durham E-Theses Aspects of structure and functionality in

w 1-·'

Figure 1. Sparging apparatus used for determining foaming prop•rties.

A = Brooks flow valve - model 8744

B =Brooks flow valve - model 8743

T = Three-way tap

N2 CYLINDER WITH HIGH PRESSURE

REDUCTION HEAD

PRESSURE GAUGE

PRESSURE REGULATOR

A

GAP FLOW METER

NEEDLE VALVE

VENT TO ATMOSPHERE

B

T

1 5.7 em

l

+--- 3 em----+ CONDUCTIVITY CELL

r- --(1 X 1 em)

1\: \: \: \:'' ' \:1--l- SAMPLE

't:t:tiWJ I SINTER (G-4)

CHART RECORDER

Page 45: Durham E-Theses Aspects of structure and functionality in

Secondly, foam expans1on (F .E.) and foam volume stability

(F.V.S.) were determined us1ng modifications of the equations

descr1bed 1n the prev1ous section.

F.E. = (1n1tial foam volume (cm 3) - 5) x 100

5

where initial foam volume is the volume of foam and liquid in

the burette 1rnmed1ately after sparging.

F .V .S. = foam volume (cm 3} after 10 min x 100

1n1tial volume of foam (cm 3 )

Where 1n1tial foam volume is defined as above.

3.8.3 compar1son Of Wh1pp1ng And Sparg1ng Methods For Determ1ning

Foam1ng Properties.

The wh1pp1ng and sparging methods were compared by the method

of least squares. Comparisons were made between a) F.E. from whlpping

exper1ments and Cl from sparging exper1ments, b) F.V.S. from wh1pp1ng

exper1ments and Co.At/Ac from sparging expenments, c) F .E. from

wh1pp1ng and sparg1ng experiments and d) F.V.S. from wh1pping and

sparging experiments for both cornmerc1ally obtained protein standards

(n = 6) and all samples tested (n = 42).

F.E. and F.V.S. from the whipp1ng method were also compared

with

a) log [AI]

where t is 0 to 0.9 ~n

and b) conduct1v1ty at 3 m1n conductlvity at 0 m1n

respect1vely (Hernmant, 1986). Compar1sons were made for a) prote1n

- 32 -

Page 46: Durham E-Theses Aspects of structure and functionality in

standards (n = 6) and b) all samples tested (n = 43).

3.8.4 Invest1gatian Of The Effect Of Sucrose On Foaming Propert1es.

The effect of sucrose on F.E., F.v.s. and F.L.S. of 0.5% (w/v)

defatted Maris Bead proteinate solut1on was determined using the

large-scale whipping method described above. Samples were either

st1rred 1n O.lM potass1um phosphate buffer, pH 7, conta1ning 0, 15, 30

or 60% (w/v) sucrose for 1 h, and foamed as previously, or sucrose (6,

12, or 24% (w/v)) was added 2 or 4 min after the start of wh1pping.

All tests were conducted 1n duplicate.

3. 9 DEI'ERMINATIOO OF EMULSIOO AcriVITY.

500 mg sample in 10 ml dist1lled water was st1rred for 1 m1n

and the pH adJusted to 7.5 w1th dilute ac1d or alkali. The rn1xture was

stirred for 1 h at roam temperature wh1lst maintain1ng the pH. 5 ml

d1spersion was added to 3 ml pure sunflower o1l 1n a 10 ml vortex

beaker and homogenized us1ng a MSE hanogenizer (Setting 2) for 20 s.

The emulsion was transferred to a 10 ml graduated centr1fuge tube and

centr1fuged in a MSE Super centrifuge at 3000 rev./min for 15 min. The

volumes ( cm 3) of free oil and emuls1on were recorded. Results were

expressed as a) ml oil absorbed/g sample and b) ml oil absorbed/g

protein. Tests were performed at least in duplicate.

3.10 DIFFERENTIAL SCANNING CAI..ORIME:l'RY.

D1tferent1al scanning calorimetry was performed us1ng a

Perkln-Elrner DSC 2B as described by Wr1ght et al. (1977). Samples were

dialyzed 1n 50mM sodium phosphate, 10% (w/v) NaCl, 1mM IJIT, 0.02%

(w/v) sod1um az1de, pH 7, and centrifuged before analys1s. Thermal

- 33 -

Page 47: Durham E-Theses Aspects of structure and functionality in

transit1ons were defined in terms of Tmax (peak temperature) and Tm

(extrapolated onset temperature). Trans1t1on enthalpies were

calculated from peak areas.

3 .11 SCANNING ELECI'RON MICROSCOPY.

Gel samples were prepared as for test1ng with the Instron

Un1versal Test1ng Machine. Preparat1on of the gels was conducted by a

modification of the method of Yasui et al. (1979). Gels were f1xed 1n

2.5% glutaraldehyde 1n O.lM phosphate buffer (pH 7) for 48 h,

post-hxed 1n OS04

for 5 h and dehydrated in an ethanol senes. After

dehydrat1on they were transferred to 50 and 100% amylacetate and

cr1t1cal po1nt dr1ed. Gels were observed with a Ph1lips 501B scann1ng

electron microscope.

- 34-

Page 48: Durham E-Theses Aspects of structure and functionality in

<liAPI'ER 4

RESULTS

4 .1 AIR ClASSIFICATION AND ANALYSIS OF FLO.JRS.

Marls Bead and IVS-G flours were analysed for moisture,

prote1n and starch contents, and the results are shown m Table 1.

Mo1sture and prote1n contents were shown to be similar, but the starch

content of IVS-G flour was lower than that of Maris Bead flour.

TABlE 1. Mo1sture, prote1n and starch contents of Marls Bead and IVS-G flours.

Mo1sture Protein Starch Sample content content content

% % %

Marls Bead

Full-fat flour 11.5 31.9 42.6

Defatted flour 5.0 32.4

- IVS-G

Full-fat flour 11.2 32.0 35.2

Defatted flour 5.2 33.2

Proteln and starch percentages were calculated on a dry we1ght bas1s.

- 35 -

Page 49: Durham E-Theses Aspects of structure and functionality in

Air classificat1on of Maris Bead and IVS-G flours y1elded the

results shown 1n Table 2. At lower speeds IVS-G gave higher y1elds of

coarse fraction than Maris Bead. Selected speeds were used to classify

IVS-G flour subJected to a second pass through a Kolloplex pin mill.

These flours gave h1gher yields of fines fraction compared to flour

subJected to a s1ngle pass through the mill (Table 2a).

TABLE 2. Alr classification of Maris Bead and IVS-G flours.

Classifier Speed Coarse Fraction Fines Fract1on

rev./min Yield (%) Yield (%)

X 1000 Maris Bead IVS-G Marls Bead

3 17.1 27.1 82.9 4 23.2 36.4 76.8 5 38.3 58.9 61.7 5.5 46.8 62.0 53.2 6 68.7 6.5 62.5 77.1 37.5 7 74.8 78.7 25.2 8 79.1 82.6 20.9 9 82.9 84.9 17.1

10 86.8 13.2 11 88.8 88.1 11.2

TABLE 2a. Air classificat1on of IVS-G flours subJected to a second pass through a Kolloplex mill.

Class1fier Speed

IVS-G

72.9 63.6 41.1 38.0 31.3 22.9 21.3 17.4 15.1

11.9

Coarse Fraction F1nes Fract1on rev./min

Yield (%) Yield (%) X 1000

3 25.1 74.9 5.5 40.7 59.3 6.5 61.8 38.2 7 65.5 34.5

Each result was produced by a s-ingle au class1flcatwn.

- 36 -

Page 50: Durham E-Theses Aspects of structure and functionality in

Percentage yield fines of air classified Maris Bead and IVS-G

flours was plotted against cut point ( m p,m) and the results are sha.ffi

in Figure 2. IVS-G flour gave lower yields of fines fraction than

Marls Bead at all cut point values. However, IVS-G flour subjected to

a second pass through the pin mill gave higher y1elds of fines

fract1on at low cut point values than Marls Bead subJected to a single

pass through the pin mill. CUt pomt was obtained from a calibration

TABLE 3. Percentage protein of a1r classified fract1ons of Marls Bead and IVS-G flours.

Prote1n (%) Class1f1er Speed

rev./mln coarse Fines

X 1000 Marls Bead IVS-G Maris Bead IVS-G .

3 18.7 15.9 29.9 37.0 4 20.6 18.0 33.2 37.9 5 22.1 24.0 38.0 41.3 5.5 19.5 19.3 39.5 53.9 6 21.0 53.8 6.5 17.0 22.1 51.2 61.5 7 19.7 22.9 58.3 65.7 8 21.4 24.1 64.2 68.0 9 21.8 24.3 67.8 70.8

10 22.9 70.9 11 23.1 25.9 75.1 74.5

TABLE 3a. Percentage protein of air classi fled fractions of IVS-G flours subJected to a second pass through a Kolloplex m11l.

Classifier Speed Prote1n (%)

rev./mln

X 1000 Coarse Fines

3 15.6 33.5 5.5 25.2 35.4 6.5 22.1 45.6 7 21.0 48.2

- 37 -

Page 51: Durham E-Theses Aspects of structure and functionality in

-'l/l. -:2 G> >. c .2

w .. co (,)

! .. CD ~ .e u.

100

90

80

70

60

50

40

30

20

10

0 0

Figure 2. Relationship between cut point and percentage fines of air-classified fractions of Marls Bead and IVS-G flours.

Maris Bead •

IVS-G •

IVS-G milled twice o

10 20 30

Cut Point (~m)

40

Page 52: Durham E-Theses Aspects of structure and functionality in

graph of classifier speed versus cut po1nt for the Alpine AlOO MZR

Z1gzag a1r classifier {Wright et al., 1984).

Protein and starch percentages of the air class1fied fract1ons

are shown in Tables 3 and 4 respectively. These results shav that

percentage prote1n in the fines fractions of Ivs-G flour was generally

greater at equivalent speeds than that of Maris Bead flour. Starch

percentages of both coarse and fines fractions of Ivs-G were lower

than those of Maris Bead w1th the exception of the fines fractions

obtained at 6500 and 7000 rev./mln.

TABLE 4. Percentage starch of air class1fied fractions of Maris Bead and IVS-G flours.

Starch {%) Classifier Speed .

rev./min Coarse Fines

X 1000 Marls Bead IVS-G MarlS Bead IVS-G

3 13.5 12.9 44.6 38.9

4 19.0 49.5

5 34.8 45.4

5.5 46.3 32.4 38.6 34.1

6.5 55.3 37.3 22.0 28.0

7 51.7 36.5 13.7 27.2

8 49.7 9.8

9 47.8 6.3

10 46.4 3.4

11 46.7 2.5

IVS-G flour was subJected to a second pass through a Ko11op1ex m1ll betore a1r classif1cat1on.

- 39 -

Page 53: Durham E-Theses Aspects of structure and functionality in

Prote1n y1elds (P.Y.) and prote1n separat1on effic1enc1es

(P.S.E.) are shown in Tables 5 and Sa. P.Y. varied from 90- 100%, but

was generally higher for IVS-G. P.S.E. was generally higher for Marls

Bead.

TABLE 5. Protein yields and protein separat1on eff1c1encies of air class1fied fractions of Maris Bead and IVS-G flours.

Class1f1er Speed Prote1n Separat1on Prote1n Y1eld

rev./nun Effic1ency

X 1000 MarlS Bead IVS-G Marls Bead IVS-G

3 100 98 90 87 4 97 96 85 80 5 100 97 73 56 5.5 94 101 71 63 6 98 55 6.5 93.5 97 67 47 7 92 100 54 44 8 95 99 47 38 9 93 98 43 36

10 92 38 11 91 99 36 29

TABLE Sa. Proteln yields and prote1n separation effic1enc1es of a1r class1fled fract1ons of IVS-G flours subJected to a second pass through a Kolloplex m1ll.

Class1f1er Speed Prote1n Separat1on

rev./nun Prote1n Yield Effic1ency

X 1000

3 91 88 5.5 98 68 6.5 97 57 7 95 57

- 40 -

Page 54: Durham E-Theses Aspects of structure and functionality in

Starch yields (S.Y.) and starch separation efficiencies

(S.S.E.) are shown in Table 6. S.Y. varied from 92 - 100%, but was

generally higher than P.Y •• S.S.E. was greater than 90% at speeds

above 6500 rev./min for Maris Bead.

Protein and starch percentages of air classified fractions

from Maris Bead and IVS-G flours were plotted against cut point in

Figures 3 and 4 respectively. Protein percentage of the fines fraction

decreased as cut point increased, but only small differences in

protein percentage of the coarse fraction at different cut points were

observed. Maris Bead and IVS-G gave similar results. Starch percentage

TABLE 6. Starch yields and starch separation efficiencies of air classified fractions of Maris Bead and IVS-G flours.

Classifier Speed . Starch Separation Starch Yield

rev./min Efficiency

X 1000 Maris Bead IVS-G Maris Bead IVS-G

3 92 92 5 9

4 100

5 97 31

5.5 99 95 51 37

6.5 100 96 79 65

7 99 95 91 68

8 97 92

9 96 93

10 96 95

11 98 98

IVS-G flour was subJected to a second pass through a Kolloplex mill before air classification.

- 41 -

Page 55: Durham E-Theses Aspects of structure and functionality in

100

90

80

70

-~ 60 -I c: ~ CD 50 N -0 ...

A. 40

30

20

10

0 0

Figure 3. Relationship between cut point and a) percentage protein and b) percentage starch of air-classified fractions of Maria Bead flour.

Fines fraction A 60 Fines fraction A

Coarse fraction 6. Coarse fraction 6.

45

-~ -s:. 30 u .. Clll .. 0

15

0+---------.-------~,-------~--------~ 10 20 30 40 0 10 20 30 40

Cut Point ( ~m) Cut Point ( ~o~m)

Page 56: Durham E-Theses Aspects of structure and functionality in

100,

90 -1

80

I 70

- 60 ~ -c

I -., 50 .J:> -w 0 ..

A. 40

30

I 20

10

.0 0

Figure 4. Relationship between cut point and a) percentage protein and b) percentage starch of air-classified fractions of IV S-G flour.

Fines fraction • 60l Fines fraction

Coarse fraction 0 Coarse fraction

'- 45

-~ -.J::. 30 CJ ..

CIIJ .. 0

~- fo-.__ 15

0 10 20 30 40 0 10 20 30

Cut Point ( ~m) Cut Point ( ~m)

• 0

40

Page 57: Durham E-Theses Aspects of structure and functionality in

ot the fines fraction Increased with increasing cut point to a maximum

at 30 p.m tor Maris Bead. Starch content of the coarse fractwn of

Maris Bead increased with increasing cut point to a maximum at 17 p.m,

and then decreased. Similar patterns were observed for IVS-G, but

fewer data points were collected.

Reclassification of Maris Bead flour subJected to a second

pass through a Kolloplex mill.

Results of the Initial classification at 6500 rev./min and the

reclassification of the coarse fraction are shown in Figure 5.

Reclassification yielded coarse fractions with up to 59.5% starch and

tines fractions with up to 60% protein.

Usually the initial and reclassified fines fract1ons are

combined to give a protein concentrate. The remaining coarse fraction

IS a starch concentrate. The yields and compos1 tions of the

concentrates are shown in Table 7. Protein and starch concentrates

with up to 57% protein and 73% starch respect1vely were produced. Low

levels of protein remained in the starch fract1on, however,

approximately 20% starch remained in the prote1n concentrate. P.S.E.

was approximately 70%, and S.S.E. was almost 80%.

Starch and protein concentrates produced at different

reclassif1cation speeds did not vary greatly in yield or compos1tion.

Generally starch content decreased and protein content increased in

both starch and protein concentrates as the reclass1f1cation speed was

increased.

- 44 -

Page 58: Durham E-Theses Aspects of structure and functionality in

+:> Vl

FIGURE 5. Reclassification of the Maris Bead coarse fraction obtained at 6500 rev./min.

T c

1st COARSE FRACTION 73.5% classification

Protein 21.1% Starch 46.2%

WHOLE BEAN FLOUR

Protein 31.9% 6500 rev./min Starch 42.6%

FINES FRACTION 26.5%

Protein 55.4% Starch 19.8%

P.Y. 95 P.S.E. 51 S.Y. 92 S.S.E. 88

he first air classification result was the average of three lassification steps.

2nd classification

5500 rev./min

.

6500 rev./min

7000 rev./min

The coarse fraction was remilled prior to the second air classification step.

COARSE FRACTION 76.7%

Protein 9.1% Starch 59.1%

FINES FRACTION 23.3%

Protein 50.7% Starch 23.2%

COARSE FRACTION 77.2%

Protein 9.6% Starch 59.5%

FINES FRACTION 22.8%

Protein 51.7% Starch 22.8% I

COARSE FRACTION 83.3%

Protein 9.9% Starch 53.9%

FINES FRACTION 16.7%

Protein 60.0% Starch 11 • 8%

P.Y. 89 P.S.E. 84 S.Y. 100 S.S.E. 79

P.Y. 90 P.S.E. 83 S.Y. 101 S.S.E. 79

P.Y. 87 P.S.E. 81 S.Y. 94 s.s.E. 84

Page 59: Durham E-Theses Aspects of structure and functionality in

TABLE 7. Yield and content of protein and produced by reclassif1cation of obtained at 6500 rev./mln.

starch concentrates the coarse fraction

Reclasslfication speed

rev./mln X 1000

5.5 6.5 7.0

PIDI'EIN CCNCENI'RATE

Yield % 43.6 43.3 38.8

Protein % 53.6 53.9 56.9

Starch % 21.1 21.0 17.3

srARCH CCNCENTRATE

Yield % 56.4 56.7 61.2

Protein % 9.1 9.6 9.9

Starch % 59.1 59.5 53.9

P.S.E. 73.2 72.9 69.2

S.S.E. 78.2 79.5 77.4

Sequent1al class1f1cation of Marls Bead and IVS-G flours.

Marls Bead and IVS-G flours were classified sequent1ally and

the results are shown in Table 8. Coarse percentage at speeds greater

than 4000 rev./min was 85 - 97%. However, at 4000 and 3000 rev./min it

was approxuately 50%. Marls Bead and IVS-G gave similar results.

Proteln percentages of the a1r classifled fract1ons are shown in Table

9. Prote1n percentage generally decreased w1th decreas1ng speed for

both coarse and f1nes fract1ons. Protein percentage of the f1nes

tract1on decreased from 75% at 11000 rev./min to approx1mately 10% at

-46-

Page 60: Durham E-Theses Aspects of structure and functionality in

TABLE 8. Sequential classification of Maris Bead and IVS-G flours.

I I I I I I I I I (%) of Initial Flour I I I

'Classifier Speedl No. Average I Average I Average I Average I I I

rev./min I of I Coarse (%) I Fines (%) I Coarse I Fines I I I I I I I

X 1000 l samples I I I I I I I I I I I I I I

lMaris Beadl IVS-G lMaris Beadl IVS-G lMaris Beadl IVS-G lMaris Beadl IVS-G I I I I I I I I I I --I I I I I I I I I I

11 I 3 I 86. 1 I 84.4 13.9 I 15.6 I 86. 1 I 84.4 I 13.9 I 15.6 I I I I I I I I I I I I I I I I I I

9 I 2 I 94.9 I 95.6 5. 1 I 4.4 I 81.7 I 80.7 I 4.4 I 3-7 I I I I I I I I I I I I I I I I

8 I 2 I 97. 1 I 97.8 2.9 2.2 I 79.3 I 78.9 I 2.4 I 1.8 I I I I I I I I I

7 I 2 I 95.7 I 96.0 I 4.3 4.0 I 75.9 I 75.7 I 3.4 I 3.2 I I I I I I I I I I I I I I I I I

.)::" I I I I I I I I I

--l I 6.5 I 2 I 95.3 I 96.3 I 4.7 3.7 I 72.3 I 72.9 I 3.6 I 2.8 I I I I I I I I I I I I I I I I

6 I 2 I 94.9 92.8 I 5. 1 7.2 I 68.6 I 67.7 I 3-7 I 5.2 I I I I I I I I I I I I I

5.5 I 2 I 89.9 89.9 10. 1 10.2 I 61.7 I 60.8 I 6.9 I 6.9 I I I I I I I I I I I I I I I

5 I 1 I 86.2 86.8 13.8 13.2 53.2 I 52.8 I 8.5 I 8.0 I I I I I

I I I I I I

4 I 1 I 54.4 55.7 45.6 I 44.4 28.9 I 29.4 I 24.3 I 23.4 I I I I I I I I I I I I I I

3 I 1 I 47.0 I 59.5 53.0 I 40.5 13.6 I 17.5 ' 15.3 I 11.9 I I I I I I I

Page 61: Durham E-Theses Aspects of structure and functionality in

TABLE 9. Percentage protein 1n sequent1ally classified fractions of Maris Bead and IVS-G flours.

Protein (%) Classifier Speed

rev./mln Coarse Fines

X 1000 Marls Bead IVS-G Maris Bead IVS~

ll 21.6 19.9 75.1 74.6

9 19.3 18.9 69.3 71.0

8 18.0 17.1 68.9 63.8

7 14.3 15.9 62.7 44.3

6.5 12.9 14.2 51.5 30.5

6 11.3 14.9 34.3 20.1

5.5 10.7 .

13.5 18.1 13.5

5 15.8 16.1 11.3 13.3

4 10.2 16.9 7.6 12.0

3 6.9 9.1 ll. 7 24.3

4000 rev ./mln for both Marls Bead and IVS-G. IVS-G gave generally

la.1er prote1n percentages 1n the fines fractions than Maris Bead,

however, at 3000 rev./min a relatively high protein percentage was

observed for IVS-G.

F1nes y1eld (%) and protein in the fines fraction (%) were

plotted aga1nst cut po1nt in Figure 6. F1nes yield was less than 16%

at cut po1nts below 30 Jlm, but protein content increased with

decreas1ng cut po1nt from a min1murn of approx1mately 10% at 30 Jlm to

75% at 10 Jlm. Marls Bead and IVS-G gave similar results.

- 48-

Page 62: Durham E-Theses Aspects of structure and functionality in

-.+== 1/l \0 -

100

90

80

70

60

50

40

30

20

Figure 6. Relationship between cut point and a) fines yield and b) fines protein percentage of sequentially air-classified fractions from Maris Bead and IVS-G flours.

Fines protein percentage (Maris Bead ) A·

Fines yield (Maris Bead) A.

Fines protein percentage (IVS-G) o

Fines yield (IVS-G) •

0+-----------------~------~----------~----------------~----------------~----

0 10 20 30 40

Cut Point ().lm)

Page 63: Durham E-Theses Aspects of structure and functionality in

4. 2 EVAIDATION OF ISOlATES, PROrEINATFS AND MICELLAR PROrEINS.

Isolates produced from Marls Bead and Ivs-G flours were soft,

creamy coloured powders. Prote1nates were darker and more fibrous. The

m1cellar proteins were creamy white powders of greater dens1ty than

the isolates. Isolates, proteinates and micellar proteins were

analysed by SDS-PAGE (Figure 7), and were shown to contain all the

maJor prote1n bands present in the respective flours. Full-fat and

defatted products were shown to have similar protein patterns on

SDS-PAGE.

Homogene1ty of isolates, proteinates and micellar proteins was

tested by using a gel flltration column of Superose 6 (Figure 8).

Elut1on prof1les of Maris Bead llS and 78 proteins are shown in F1gure

ll. The samples were shown to d1ffer with respect to protein

aggregat1on, as determined by the amount of h1gh molecular weight

mater1al (retention t1me of approximately 20 min), and the amount of

low molecular we1ght material (retention time greater than 50 min).

The defatted isolate and micellar proteins had the largest and

smallest peaks designated to conta1n material of an approx1mate Mr. of

3000 x 103

respectively. Isolates and proteinates both showed large

peaks of mater1al w1th a Mr. of < 5000, but only small corresponding

peaks were observed for the m1cellar prote1ns.

Protein contents of isolates, proteinates and m1cellar

proteins are shown in Table 10. Full-fat samples had protein contents

2 - 4% lower than defatted samples. M1cellar prote1ns had the highest

prote1n content, and prote1nates the lowest protein content. Us1ng a

n1trogen to protein conversion factor ot 6.25 gives very h1gh values

of protein percentage as it is an average value for all proteins. A

factor of 5.7 1s generally used for Vlcia faba prote1ns, and g1ves

- 50 -

Page 64: Durham E-Theses Aspects of structure and functionality in

F'gure 7. SDS-PAGE of proteins extracted from flours, i so l a tes, pro e · na es and micellar pro eins.

Track Sample

Standards

2 IVS-G flour

3 Maris Bead proteinate

M r .1 o-3

Q2

67

45

35

25

21

18.5

12.5

5

6

2 3

- 5

Maris Bead isolate

Maris Bead micellar pro

Maris Bead lour

ein

1 r 1 • lii

ubun1t

Page 65: Durham E-Theses Aspects of structure and functionality in

Figure 8. Elution profiles of isolates, proteinates, and micellar proteins from Maris Bead after gel filtration chromatography on Superose 6.

0.5 A 4 8

2 5

0.4 1

0.3

0.2

7

0 1 0 20 30 40 50 60 10 20 30 ~0 50 60 70 0.5

-eo.4 ...... Cl E -.!:o.3 «» ... 0 ... Q.

0.2

c

0

0.5 E

.0.4

0.3

0.2

10 20 30 40 17

11

50 60

D

F

13 15

10 20 30 40 50 60 70

21

. 0 10 20 30 40 50 60 10 20 30 40 50 60 70 Time (min) ·

Page 66: Durham E-Theses Aspects of structure and functionality in

SAMPlE

A. Defatted 1solate B. Full-fat 1solate c. Defatted proteinate D. Full-fat proteinate E. Defatted m1cellar protein F. Full-fat m1cellar prote1n

From a calibration graph the peaks were des1gnated to contain rnater1al of IIDlecular weights as ind1cated (Lambert, 1986) .

Peak No. Retention Time Mr. X 10-3

(m1n)

1 20 3000 2 39 200 3 47 16 4 59 <5 5 39 200 6 47 16 7 57 <5 8 20 3000 9 40 150

10 47 16 11 57 <5 12 20 3000 13 39 200 14 48 15 15 58 <5 16 20 3000 17 39 200 18 48 15 19 58 <5 20 20 3000 21 38 350 22 47 16 23 58 <5

Load1ng was 1 rng in 100 ~-Mlcellar proteins were produced by ultrafiltration.

- 52-

Page 67: Durham E-Theses Aspects of structure and functionality in

TABLE 10. Protein contents of isolates, proteinates and micellar proteins.

Protein (%) Sample N X 6.25

Maris Bead

Full-fat proteinate 86.6

Defatted proteinate 90.6

Full-fat isolate 89.8

Defatted isolate 94.2

Full-fat micellar protein 105.8

Defatted micellar protein 107.8

IVS-G

Full-fat proteinate 89.7

Defatted proteinate 91.6

Full-fat isolate 93.2

Defatted isolate 96.9

Defatted micellar protein 107.8

average protein contents of 83.1%, 87.1% and 98.3% for the defatted

proteinates, Isolates and micellar prote1ns respectively. However, to

facilitate comparison with the literature a value of 6.25 has been

used.

4.3 PURIFICATION AND ANALYSIS OF PROTEINS.

Separation of globulins on HA-Ultrogel yielded the elution

profile shown In Figure 9. Legumin was represented by the flrst,

larger peak and vicilln by the second and broader peak. A region where

both proteins occurred was found between. The fractions were analysed

by SDS~PAGE (Figure 10). MaJor protein bands were observed

- 53 -

Page 68: Durham E-Theses Aspects of structure and functionality in

8

7

6

e c 0 CD 5 N -" >-!! Cl)

4 c • , " u ;: Q. 3 0

2

1

0 70

Figure 9. Elution profile of crude globulins

from Maris Bead on HA- Ultrogel.

Elution was performed using a linear concentration gradient of potassium phosphate buffer, pH 7.8 (50mM - 0.75M, 500 ml + 500 ml).

80 90 100 110 120

Fraction number

- 54 -

130 140

Page 69: Durham E-Theses Aspects of structure and functionality in

Figure 10. SDS-PAGE of legumin and vicilin from Maris Bead seeds .

87

45

35

26

21 18 .6

Track

2

3

Sample

Vicilin

Legumin

Legumin ( + mercap oe ano )

1 2 3

- 55 -

Page 70: Durham E-Theses Aspects of structure and functionality in

corresponding to molecular we1ghts of 56 000 and 40 000 on non-reduced

gels and 36 000, 23 000 and 21 000 on reduced gels for llS proteins,

and 66 000, 60 000, 55 000 and 38 000 for 7S proteins. Marls Bead and

IVS-G prote1ns gave sinular patterns on SDS-PAGE. Fractions showing

leguman w1thout contaminat1ng vicilin, or vice versa, were kept for

subsequent experiments. The prote1ns were tested for horrogene1 ty on a

gel f1ltration column of Superose 6 and us1ng an analytical scann1ng

ultracentrifuge (Figures ll and 12 respect1vely}. On Superose 6

v1c1lin gave a single peak with a retention t1me of 42 min. It was

des1gnated to conta1n mater1al of an approximate Mr. of 100 x 10 3

Legum1n yielded three peaks designated to contain mater1al of

approx1mate Mr. values of 3 nullion, 600 000 and 300 000. The former

peak was larger if llS prote1ns were d1alyzed against dist1lled water

than 1f they were dialyzed aga1nst ammonlUm hydrogen carbonate. Us1ng

the analyt1cal ultracentr1fuge the llS prote1n y1elded a small peak

w1th an Sobs value of 14 - 16 and a larger peak. Vlcilin gave a

s1ngle, broad peak. S~ 0 ,w values are shown in Table ll.

TABLE 11. Sed1mentat1on coeff1cients of llS and 7S proteins.

0 S2o 'W

Sample Marls Bead IVS-G

us 11.3 ll. 7

7 s 7.4 7.3

- 56 -

Page 71: Durham E-Theses Aspects of structure and functionality in

SAMPLE

A. Maris Bead vicilin

B. Maris Bead legumin - dialyzed against distilled water

C. Maris Bead legumin - dialyzed against ammonium hydrogen carbonate

Peak No. I Retention Time I Mr. x 10-3 I I

(min)

--42 I 100 I

I I I I I I I

Vl I 2 I 20 I 3000 --l I I I

3 I 34 I 600 I I I I

4 I 38 I 300 I I I I

5 I 20 I 3000 I I I I I I

6 I 34 I 600 I I

7 I 38 I 300 I I

Page 72: Durham E-Theses Aspects of structure and functionality in

-i :II :IIIII .. s .a .. • -c: 0 -.. ! .. c: • 0 c: 0 0

.5 • .. 0 .. ~

-CD !:: c: :I :IIIII .. ftJ .. !:: .a .. ca -c: 0 -.. ca .. ... c ~ u c 0 0

.5 ., .. 0 .. ~

Figure 12. Analytical scanning ultracentr:lfugatlon of 11 S and 7S proteins from Marls Bead.

1. 11 S. 2% solution after 40 min. 9

8

7

6

5

4

3

2

1

0

0 20 40 60 80 100 120 140 160 180 200 220 Distance (mm)

2. 7S. 1.5% solution after 55 min. 9

8

7

6

5

4

3

2

1

0

0 20 40 60 80 100 120 140 160 180 200 220

Distance {mm)

- 58 -

Page 73: Durham E-Theses Aspects of structure and functionality in

4.4 DISPERSIBILITY AND GELLIOO CHARACI'ERisriCS OF ISOLATES,

PROI'EINATES AND MICEIJAR PRCYI'EINS.

Dispersibility and gelling characteristics of Marls Bead and

IVS-G proteinates and micellar proteins with respect to pH are shown

in F1gures 13 - 18. Protein solubility and turbidity of the same

samples are shown in Figures 19 - 22. Sediment volume was used as a

measure of dispersibility, and non-dispersed material was assumed to

be composed of protein aggregates.

Sediment volumes of proteinates were generally highest at

pH 3.5 and 6, and lowest at pH values of <3 and >6. The full-fat Maris

Bead proteinate did not give a peak at pH 6 but as fewer data po1nts

were collected this may have been missed. Micellar proteins gave

similar results but the volumes of sediment were lower. This did not

reflect a greater dispersibility, as can be seen from the protein

solubility graphs for defatted IVS-G proteinate and micellar protein

(Figures 19 and 22). The proteinate had approximately 10% more protein

1n solution despite having an original protein content of 15% less

than the micellar protein. Turbidity was also lower for the micellar

protein. Volume of sediment can not be taken as an absolute measure of

disperslbility as it is affected by the nature of the sample and pH

value. These results show sediment volume Is negatively correlated

w1th protein content of the supernatant and turbidity over a pH range

for each sample tested. It is, therefore, a quick and useful

assessment of d1spers1b1lity of a particular sample at various pH

values, but of less use for comparing dissimilar samples.

Gels were formed from 10% solutfons of defatted and full-fat

prote1nates at pH values of 2- 3.5 and 6- 7, and at 3.5- 4 and >7

for micellar proteins. The 20% defatted IVS-G proteinate gelled over a

- 59 -

Page 74: Durham E-Theses Aspects of structure and functionality in

Figure 13. Diaperalbllity and gelling characteristics of defatted Maria Bead proteinate ( 1 0~ solution).

Page 75: Durham E-Theses Aspects of structure and functionality in

8

7

6

-(') 5 E

"' (,) ..... -~ 4

.2 0 3 >

2-i I

I I 1

0 1 2

Figure 14. Dispersibility and gelling characteristics of defatted IVS-G proteinate ( 1 0% solution).

Sediment Gel

4

:1( 2

CD , c 0 -CD

• " -2

-4- . '

_/ \ \1 I I 2 4 6 pH

/ L 1\ I

3 4 5 6 1 8 9 10

pH

• 0

' ' 8 10

1 1

Page 76: Durham E-Theses Aspects of structure and functionality in

Figure 15. Dlsperslbility and gelling characteristics of defatted IVS-G proteinate (20% solution) ..

Page 77: Durham E-Theses Aspects of structure and functionality in

8

7

I 6

-(I) 5 E 0'\ Q w -I 4 .a 0 3 >

21 1/ 1

0 1 2

Figure 16. Diaperslblllty and gelling characteristics of full-fat Marla Bead proteinate ( 1 0% solution).

Sediment

Gel

1\ I 4

II( 2 • '0 .s 0 "i

" -2

-4-4

\ ~ \ I 2

pH

3 4 5 6 7 8 9 10

pH

&

1:.

68 10

11

Page 78: Durham E-Theses Aspects of structure and functionality in

Figure 17. Dlsperslbillty and geJIIng characteristics of defatted Marls Bead micellar protein ( 1 0% solution).

Sediment •

Gel 6.

Page 79: Durham E-Theses Aspects of structure and functionality in

Figure 18. DlsperslbUity and geJIIng characteristics of defatted IVS-G micellar protein ( 1 0" solution).

Page 80: Durham E-Theses Aspects of structure and functionality in

Figure 19. Protein solubility of defatted IVS-G proteinate ( 1 0.., solution).

100l 15

90 -i 80 4 ........

0) -e e - c ... 70 0 c ., "' .... .. i 60 3 -.,

Q 50 0 -"' - >-

"' 0 = ... 40 2 'a c .! :a .. c :::» 0 30 ... ()

Jii

201 -

' _ __1 Protein content ! 0 f-1 0 ...

Turbidity 0. • 10 -

0 0 1 2 3 4 5 6 7 8 9 10 11

pH

Page 81: Durham E-Theses Aspects of structure and functionality in

Figure 20. Protein solubility of ful-fat Maris Bead proteinate ( 1 0% solution).

100l .......

15

90 -e 80 4 ....... ., -E E - c .... 70 0 c • C'l .. ..

I 60 3 ... • Q

50 0 -"' - "' -..;J 0 :t: c 40 Protein content

2 , • :a g ..

Single layer • :::J

c.» 30 ... .5i Top layer 0 ! 20 ~1 0 Second layer A .. CL

10 Turbidity ... 0 0

1 2 3 4 5 6 7 8 9 10 11

pH

Page 82: Durham E-Theses Aspects of structure and functionality in

Figure 21. Protein solubility of defatted Maris Bead micellar protein ( 1 0~ solution).

100l 15

90 -e 80 -...... 4

0) -E I -.. 70 0 C. .s N

I 60 ~

3 ... .. Q

50 0 -"' - >-CD 0

1 40 ~

2 :!! ~

i .. 30

:::s c,) .J:. ... .. .! 20 ~1 0 .. Protein content 1::.. 111.

10 Turbidity .&

0 0 1 2 3 4 5 6 7 8 9 10 11

pH

Page 83: Durham E-Theses Aspects of structure and functionality in

100l

90 -e 80 ' c.

e -- 70 c Cl -I 60

50 0\ ... \.0 0

i 40

g u 30 .s

201 ! 0 ... G,.

10

0 1 2

Figure 22. Protein solubility of defatted IVS-G micellar protein ( 1 0% solution) .

.

\ ~ --~ Protein content 0

Turbidity •

3 4 5 6 7 8 9 10

pH

15

4 -e c 0 ~ ..

3 -• Q 0 -"" = 2 'V 1i .. :s 1-

l-1

0 11

Page 84: Durham E-Theses Aspects of structure and functionality in

broader pH range, i.e. 2 3.5 and 6.5 - 9. Gel volume is also

affected by the nature of the sample and pH. Structural differences

were reflected in the varied physical appearance of gels with respect

to pH. At pH values of 3. 5 and 6 - 7 gels were generally opaque and

pasty. At other pH values they were less granular and often

translucent. The former attained higher values on the gel index.

Protein solubility and turbidity were generally well

correlated (F1gures 19- 22), and negatively correlated w1th volume of

sedunent. They were h1gh at pH values between 2 - 3. 5 and >6. Prote1n

contents at the above pH values were approximately 80% for

prote1nates, 65% for IVS-G micellar prote1n and <35% for Marls Bead

m1cellar prote1n.

The full-fat Maris Bead prote1nate behaved in a different

manner to the other samples, forming three layers in the test-tube

after the first centrifugation at some pH values. The bottom layer was

a solid precip1tate, the second layer an opaque collo1d accounting for

50 - 75% of the total volume, and the third layer a clear solut1on

account1ng for 7 - 20% of the total volume. After heating at 95°C two

d1st1nct regions of gel were observed. The top layer was translucent

whilst the bottom layer was opaque and very granular. They exhibited

s1milar gel 1nd1ces. Prior to gell1ng a sample of solution was taken

from both layers and analysed for nitrogen content. Both values are

plotted 1n F1gure 20. The turbidity values refer only to the colloidal

layer at those pH values where three layers were formed. A colloid was

not formed at pH values of 4, 5, 7 or 8.

The effect of salt on the gel index, dispersibllity and

gelling character1st1cs of defatted Marls Bead proteinate (pH 7.7) is

shown 1n F1gure 23. Protein solubility and turbidity are plotted

- 70 -

Page 85: Durham E-Theses Aspects of structure and functionality in

aga1.nst salt content 1.n Figure 24. Sediment volume was low at all salt

concentrations, but a small increase with increasing salt content was

observed. Weak gels were formed at salt concentrations between 0. 5 and

1. 5%. Protein content of the supernatant generally decreased with

increasing salt content. The supernatants were dark in colour at all

pH values, which interfered with the turbidity readings. However, the

supernatants were translucent at all salt concentrations with the

except1.on of 1.5 and 1.75%.

Compression and stress relaxation propert1.es of gels.

Values of G, n and rupture strength obta1.ned from un1.ax1.al

compression exper1.ments on 20% gels of Maris Bead and IVS-G

protel.nates, isolates and micellar proteins are shown in Table 12.

Values of G ranged from 0.2g - -2 1.76 kgrrnn Defatted

proteinates (pH 7) generally gave a lower value of G than defatted

micellar proteins (pH 7). G was large for samples gelled at pH 4.

Values of n ranged from 0.13 - 1.50. IVS-G proteinates gave higher

values of n than Maris Bead proteinates. At pH 4 lower values of n

were observed compared to equivalent samples at pH 7. Rupture strength

was greatest for the full-fat Maris Bead isolate (pH 4.6). Defatted

IVS-G m1.cellar prote1.n and prote1.nate (pH 7) gave similar values, as

d1.d defatted Maris Bead micellar protein and proteinate (pH 7).

Protein contents of the 20% solutions after centrifug1.ng and

pH correctl.on, but prior to gelling are shown in Table 13. Prote1.n

concentrations were 15 - 16% for proteinates, 11 - 12% for full-fat

1.solates and 8.5 - 12.5% for defatted micellar proteins. The samples

prepared for scanning electron microscopy had lower prote1.n contents.

- 71 -

Page 86: Durham E-Theses Aspects of structure and functionality in

8

7

6

-..,E 5 u

-.:1 -1\) • 4 E ::9 0

3 >

2

1

0 0 0.25

Figure 23. Effect of salt on the dlsperalblllty and gelling characteristics of defatted Marls Bead proteinate ( 1 0% solution at pH 7. 7) .

0.5 0.75 1.0 1.25 1.5 1.75

tKt Salt

4

2 »C •

Sediment •

Gel 6.

~ 0 .J_ ____ -/ -"i CJ -2

-4 o-~ Salt

2.0

Page 87: Durham E-Theses Aspects of structure and functionality in

100-, ~

90 -e ' 80 CJ)

E -- 70 c G -ftJ 60 E ~ 50 a»

--.J -w 0 - 40 c ~ -c 0 30 u .e • 20 -0 .. A.

10

0 0

Figure 24. Effect of salt on protein solubility of defatted Marla Bead proteinate ( 1 0% solution) .

Protein content

Turbidity

0.25 0.5 0.75 1.0 1.25 1.5 1.75 2.0

%Salt

1::.

2.25

r5

4 -E c 0 N ..

3 -G

Q 0 ->-:!:::

2 :!! &J .. ::::s ...

~1

0

Page 88: Durham E-Theses Aspects of structure and functionality in

TABLE 12. Uniaxial compression of isolate, proteinate and micellar protein gels.

No. of G Rupture Sample ffl Kg mm- 2 n strength

Samples X 10-4 Nm- 2

MB proteinate 7 4 1. 76 0.83 1500 - full-fat +0.21 +0. 28 +130 - - -

MB proteinate 7.4 2 0.57 0.96 600 - defatted +0.21 +0.07 +90 - - -

IVS-G proteinate 7 4 0.66 1.50 840 - defatted +0.08 +() .14 +70

- - -

IVS-G proteinate 7.7 2 1.07 1.35 1040 - defatted +0.25 +0.36 +140 - - -

MB Isolate 7 3 0.29 1.19 290 - full-fat +0.07 +0.06 +20

- - -

MB 1solate 4.6 4 1.62 0.78 2130 - full-fat +0.06 +0.09 +830 - - -

MB micellar protein 7 4 1.12 0.66 830 - full-fat +0.39 +0.21 +220

- - -

M3 micellar protein 4 2 1. 70 0.13 933 - defatted +0.08 +0. 24 +50

- - -

MB m1cellar protein 7 6 0.61 0.92 610 - defatted +0.16 +() .42 +250

- - -

IVS-G micellar 7 6 1.62 0.92 1080 prote1n - defatted +0. 21 +0.19 +370

- - -

MB = Marls Bead

The gels varied greatly in appearance. At pH 7 prote1nates and

Isolates generally formed dark coloured, semi-translucent gels that

were springy to the touch. At pH 4.6 the isolate formed a lighter

coloured, pasty gel which exhibited syneresis. The micellar proteins

formed gels with the rrost pasty appearance, particularly at pH 4 where

syneresis was also observed. Scanning electron micrographs of 20% gels

of defatted Marls Bead Isolate, proteinate and micellar proteln are

- 74 -

Page 89: Durham E-Theses Aspects of structure and functionality in

TABLE 13. Protein contents of 20% solutions prior to gell1ng.

Sample Protein Content (%)

MB proteinate - full-fat - pH 7 15.6

MB prote1nate- defatted- pH 7.4 15.9

IVS-G proteinate - defatted - pH 7 15.8

MB isolate - full-fat - pH 7 11.2

MB 1solate - full-fat - pH 4.6 12.0

MB micellar prote1n - defatted - pH 4 8.6

MB m1cellar protein - defatted - pH 7 10.4

IVS-G micellar protein -defatted pH 7 12.4

SEM Samples

MB proteinate - defatted - pH 7 10.8

MB 1solate - defatted - pH 7 11.3

MB micellar protein - defatted - pH 7 8.6

MB = Maris Bead

shown in Figure 25. Dlfferences in structure were observed. The

prote1nate and 1solate had coarser internal structures than the

m1cellar protein, reflecting a greater extent of protein aggregat1on.

Relaxat1on times and peak he1ghts from stress relaxation

exper1ments on 20% gels are shown in Table 14. Relaxat1on t1mes were

of the order 0.8 s, 8 s and 90 s for prote1nates, 0.3 s, 3 s and 25 s

tor 1solates and 0.8 s, 7 s and 50 s for micellar proteins. Generally

the slowest relaxat1on time gave the largest peak he1ght (~) for the

prote1nates, although this was not ruch larger than A2

• A1

was

approx1mately 65% of e1 ther of the other two peak heights. The peak

heights of the slowest relaxation t1me for the isolates and m1cellar

- 75 -

Page 90: Durham E-Theses Aspects of structure and functionality in

A

B

c

Page 91: Durham E-Theses Aspects of structure and functionality in

F1gure 25. Scann1ng electron micrographs of gels of Maris Bead 1solate, proteinate and m1cellar protein.

A. Defatted Marls Bead isolate

B. Defatted Maris Bead proteinate

C. Defatted Marls Bead micellar prote1n

Magnificat1on factor was x20 000.

All gels were produced from 20% solutions at pH 7.

- 76 -

Page 92: Durham E-Theses Aspects of structure and functionality in

TABLE 14. Relaxation t1mes of 1solate, proteinate and micellar protein gels.

* results of only one sample tested

Relaxation time Peak Height Strain s X 10- 3 N

Sample pH %

1 2 3 A1 A AJ 2

--MB proteinate 6.9 10 0.49 4.2 35 41 56 63

- full-fat 20 0.72 5.7 70 122 177 1% 30 0.74 6.6 74 195 246 261

MB proteinate 7.0 10 0.54 5.0 45 47 69 73 - full-fat 20 0.94 8.9 89 151 201 202

30 0.76 7.7 96 211 276 276

MB proteinate 6.9 10 0.69 6.9 70 53 81 81 - defatted 20 0. 79 7.2 70 93 184 229

30 1.00 9.8 106 171 230 263

IVS-G proteinate 6.6 10 0.58 5.7 52 56 79 75 - defatted 20 0. 71 6.5 66 110 143 149

IVS-G prote1nate 7.0 10 0.65 6.4 33 32 34 36 - defatted 20 0.64 6.0 69 91 121 120

30 0.79 7.7 81 116 152 233

MB 1solate 7.0 10* 0.41 3.0 25 62 86 98 - full-fat 30 0.32 2.0 17 167 215 115

MB isolate 4.6 10* 0.31 3.3 33 199 192 154 - full-fat 15* 0.31 2.9 29 178 184 156

20* 0.25 2.0 18 100 105 99

MB micellar prote1n 7.0 10 0.66 6.0 50 17 24 21 - full-fat 20 0.76 6.2 57 52 65 51

MB micellar protein 4.0 10* 0.71 7.5 8.8 97 125 139 - defatted 20* 0.48 2.9 16.9 119 189 305

MB m1cellar protein 7.0 10* 1.0 9.4 68 41 43 21 - defatted 20* 0.43 3.1 27 105 158 196

30* 0.49 4.5 54 151 206 237

IVS-G micellar 7.0 10 0.43 5.0 53 34 50 37 prote1n - defatted 20 0. 77 7.4 77 99 139 146

30 0.85 7.9 106 160 205 254

-- --

MB = Marls Bead

- 77 -

Page 93: Durham E-Theses Aspects of structure and functionality in

prote1ns were proportionally less 1n some instances. From these

samples there was no clear pattern.

Co-operat1ve flow analysis of the same samples y1elded the

results shown in Table 15. Co-ordination m.unber, z, generally

1ncreased w1th increasing compressive strain. For proteinates the

co-ord1nat1on number was ~igher (3 4) than for 1solates

(approximately 2).

Samples were tested in dupl1cate or tr1plicate unless

otherw1se 1nd1cated.

TABLE 15. Co-ordination number of the first flow process in gels subJected to stress relaxation experiments.

I Co-ordinatlon Intercept

Strain Sample pH Number Wlth F/F~

% z ax1s

MB prote1nate 6.9 10 3.2 0.25 - full-fat 30 3.9 0.22

MB proteinate 7.0 20 2.3 0.39 - full-fat 30 3.2 0.24

MB prote1nate 7.0 10 3.4 0.35 - defatted 20 2.5 0.45

30 4.3 0.25

IVS-G prote1nate 6.6 10 1.4 0.47 - defatted 20 1.8 0.42

IVS-G prote1nate 7.0 10 2.2 0.01 - defatted 20 3.9 0.12

30 2.9 0.01

MB 1solate 7.0 10 1.8 0.29 - full-fat

MB isolate 4.6 10 1.3 0.45 - full-fat 15 1.5 0.43

20 2.2 0.28

MB = Marls Bead

- 78 -

I I

Page 94: Durham E-Theses Aspects of structure and functionality in

4. 5 ASSESSMENT OF FOAMING ABILITY

Foaming ability was assessed by two contrasting methods: a) a

large scale whipping method and b) a small scale conduct1vity method.

The results are sununarised in Table 16. BSA, hemoglobin, sodium

case1nate and soy whey protein produced the highest values of F.E. and

F.V.S. obta1ned by the whipping method, whilst a-casein, sodll.lm

caseinate, soy whey protein, spray dried egg white and BSA produced

the highest in1t1al conductivitles in the sparg1ng experiments. The

two methods d1d not produce the same rank1ng order for foam expansion

or foam stability. In the whipping experiments lysozyme, full-fat soy

flour and Fllby micellar protein produced the lowest values of F.E.

and F.V.S •. However, flours and air classifled fractions were the

poorest foaming agents as JUdged by init1al conduct1vity and the foam

stability index (Co~t/~) in the sparg1ng experiments.

There was little variation in F.E. determined by the sparging

exper1ments, despite a ten fold variation observed in the whipp1ng

exper1ments. F.V.S. from the sparg1ng experiments varied from 7.5 for

lysozyme to 74.8 for defatted soy flour.

Values of F.L.S. determined by both methods were low. The bulk

of the solut1on incorporated in the foam during whipp1ng or sparging

dra1ns very qu1ckly after foaming is completed. Subsequent changes in

liquid volume are small. This makes F.L.S. a relat1vely insensltive

measure of foam stability. -y--globulin had the greatest and II1Y03lobin

the lowest foam expansion as determined by log (initial rate of fall

1n conductiv1ty). Foam volume stabllity (determined by div1ding

conductlvity after 3 m1n by init1al conductiv1ty) was high for sodium

caseinate, BSA and soy whey protein, and lo.v for lysozyme and

myoglobin.

- 79 -

Page 95: Durham E-Theses Aspects of structure and functionality in

TABLE 16. Foarn1ng abillty from wh1pp1ng and sparg1ng expenrnents.

WHIPPING SPARGING

SAMPLE F.E. F.V.S. F.L.S. Cl

mS em -1

Lysozyme 52 + 0 14.2 + 2.2 11.2 + 0 0.75 + 0.02 - - - -

Hernog1obln 575 + 19.8 82.8 + 3.3 15.8 + 7.4 1.13 + 0.13 - - - -

')'-globulln 252 + 23.4 76.9 + 3.1 18.4 + 4.0 0.94 + 0.02 - - - -

Myoglob1n 236 + 0 49.1 + 1.6 10.4 + 2.3 1.49 + 0.12 - - - -

BSA 588 + 13.9 90.1 + 0 32.0 + 6.9 1.62 + 0.17 - - - -

Ovalburnln 1.21 + 0.12 -

Sod1um case1nate 522 + 4.0 85.3 + 3.1 21.3 + 1.2 2.06 + 0.15 - - - -

{3-lactog1obulln 0.77 + 0.02 -

~-case1n 2.13 + 0.01 -

Marls Bead llS 1.06 + 0.1 -

Marls Bead 7 s 1.40 + 0.01 -

IVS~ llS l. 23 + 0.08 -

IVS~ 7 s 0.87 + 0.04 -

Bute 7 s 1.19 + 0.06 -

Bute globul1ns 1.48 + 0.05 -

B1rte llS 1.49 + 0.01 -

Renwh1tes 414 + 19.8 81.0 + 1.5 18.0 + 0 1.67 + 0.13 - - - -

F1lby whey protein l. 22 + 0.02 -

Soy whey prote1n 548+ 0 79.2 + 0.6 15.2 + 1.1 1.80 + 0.05 - - - -

Soy concentrate 204 + 0 69.8 + 0.09 12.2 +-0.3 1.13 + 0.06 - - - -

Page 96: Durham E-Theses Aspects of structure and functionality in

SPARGING

Co.& /de F.E. F.v.s. F.L.S. 103 ~~]* C 3min

Ci

0.4 146 7.5 7.9 -0.14 0.03

5.1 143 64.3 27.6 -0.26 0.24

-0.44 0.43 I

4.3 154 42.0 11.8 -0.01 0.10 I

6.7 147 65.3 22.4 -0.29 0.42

7.3 -0.20 0.46

7.9 136 72.6 25.0

10.7 149 73.6 28.1

9.3 137 73.0 26.3

8.1 154 71.4 35.1

10.0 145 69.4 22.4

8.1

7.6 150 70.0 26.3

8.8 150 71.1 28.9

7.6 -0.31 0.41

8.3

6.8 153 72.0 30.3 -0.26 0.42

5.7 161 66.7 22.8 -0.23 0.24

* t 15 0 - 0.9 m1n.

- 80 -

Page 97: Durham E-Theses Aspects of structure and functionality in

TABLE 16 cont1nued.

WHIPPING SPARGING

SAMPLE F.E. F.V.S. F.L.S. Cl

mS cm- 1

Soy meal - defatted 426 + 2.8 85.1 + 0.5 23.4 + 0.8 1.19 + 0.06 - - - -

Soy meal - full-fat 42 + 2.8 20.0 + 0 4.0 + 0 1.14 + 0.2 - - - -

Soy 1solate 446+ 8.5 84.3 + 1.3 21.0 + 1.4 1.21 + 0.05 - - - -

Marls Bead proteinate 156 + 5.7 63.5 + 0.5 ll.6 + 0.6 1.23 + 0.03 - - - -

- full-fat Marls Bead proteinate 314 + 2.0 80.0 + 1.4 21.2 + 0.6 1.22 + 0.03

- - - -- defatted

Marls Bead 1solate 122 + 2.8 57.8 + 0.1 7.2 + 0 0.87 + 0.03 - - - -

- full-fat Marls Bead 1solate 335 + 39.9 79.8 + 3.0 15.6 + 2.1 1.14 + 0.03

- - - -- defatted

IVS-G proteinate 150 + 2.8 53.0 + 0.3 4.6 + 0.8 0.91 + 0 - - - -

- full-fat IVS-G proteinate 254 + 19.8 74.9 + 2.1 13.4 + 0.3 1.19 + 0

- - - -- defatted

IVS-G 1solate 221 + 1.4 65.7 + 0.7 5.0 + 0.3 0.91 + 0.01 - - - -

- full-tat . IVS-G 1solate 262 + 8.2 75.2 + 0.8 10.9 + 1.2 1.16 + 0.02

- - - -- defatted

Marls Bead m1cellar 178 + 8.5 69.4 + 0.4 15.0 + 1.4 1.15 + 0.03 - - - -

prote1n - full-fat Marls Bead m1cellar 275 + 14.0 76.8 + 0.3 13.7 + 2.1 1.21 + 0.04

- - - -prote1n - defatted

IVS-G m1cellar prote1n 0.50 + 0.03 -- defatted

F1lby proteinate 164 + 0 49.6 + 2.2 3.0 + 0.3 1.13 + 0.04 - - - -

- full-fat Fllby lSOlate 152 + 2.8 50.7 + 4.9 5.8 + 2.5 1.02 + 0.04

- - - -- full-fat

F1lby m1cellar prote1n 76 + 0 31.7 + 0.8 4.8 + 0 0.81 + 0 - - - -

- full-fat Progreta Proteinate 310 + 8.5 78.7 + 0.9 17.8+1.4 1.14 + 0.02

- - - -- defatted

Progreta isolate 239 + 4.6 70.1 + 1.8 10.7 + 2.3 1.09 + 0 - - - -

- full-fat

Micellar proteins were prepared by ultrafiltration.

Page 98: Durham E-Theses Aspects of structure and functionality in

--- ·---

SPARGING

co.At /de F.E. F.V.S. F.L.S. 1CXJ ~~] * C 3mm

Cl

7.4 168 74.8 23.7 -0.35 0.41

5.7 140 59.9 16.3 -0.24 0.25

7.6 154 68.9 21.1 -0.34 0.41

7.2 -0.34 0.40

7.8 -0.35 0.41

6.6 -0.41 0.32

7.4 -0.37 0.40 .

6.9 147 67.6 17.1 -0.37 0.32

5.6 -0.27 0.27

5.2 146 60.4 5.2 -0.21 0.15

6.6 149 66.7 13.2 -0.31 0.35

7.7 146 72.7 36.8 -0.40 0.43

7.6 149 70.6 23.0 -0.34 0.40

5.3 138 42.5 15.8 -0.18 0.20

5.2 154 24.9 12.5 -0.24 0.21

5.8 150 57.9 13.2 -0.32 0.22

7.4 147 67.3 21.9 -0.34 0.39

6.1 155 70.1 21.1 -0.34 0.33

- --

* t 1s 0 - 0.9 m1n.

- 81 -

Page 99: Durham E-Theses Aspects of structure and functionality in

TABLE 16 cont1nued.

WHIPPING SPARGING

SAMPLE F.E. F.V.S. F.L.S. Cl

mS em _,

Progreta isolate 452 + 11.3 85.3 + 0.3 18.6 + 0.3 1.37 + 0.06 - - - -- defatted

F1eld bean prote1nate 379 + 4.2 83.4 + 1.1 22.6 + 7.6 1.31 + 0.08 - - - -- detatted

Marls Bead flour 162 + 2.8 46.3 + 1.3 4.4 + 0.6 0.29 + 0.02 - - - -- full-fat

Marls Bead flour 236 + 5.7 72.8 + 1.8 10.8 + 1.7 0.84 + 0.11 - - - -

- defatted IVS-G flour 160 + 5.7 55.6 + 1.0 3.4 + 0.8 0.38 + 0

- - - -- full-fat

IVS-G flour 181 + 4.2 66.1 + 0.3 6.8 + 2.3 0.66 + 0 - - - -- defatted

F1lby pea flour 205 + 9.8 68.8 + l. 7 8.9 + 1.8 0. 77 + 0.04 - - - -

- detatted F1lby pea flour rn1lled 236 + 8.5 67.4 + 0.1 5.6 + l. 7 0.41 + 0.02

- - -tw1ce - detatted

AIR-cLASSIFIED FRACI'IONS .

Marls Bead 3 c 14 + 2.8 6.3 + 0.8 2.2 + 0.3 0.15 + 0.07 - - - -

IVS-G 3 c 146 + 25.5 42.0 +12.7 4.3 + 0.6 0.2 + 0 - - - -

Marls Bead 6.5 c 125 + 1.4 so. 7 + 1.4 4.0 + 1.1 0.2 + 0 - - - -

IVS-G 7 c 148 + 0 47.3 + 1.4 1.2 + 0.6 0.22 + 0.03 - - - -

Marls Bead 7 F 162 + 2.8 57.1 + 1.5 4.6 + 1.4 0.47 + 0.03 - - - -

IVS-G 7 F 179 + 9.9 59.0 + 0.2 2.6 + 0.3 0.39 + 0.03 - - - -

Marls Bead 11 F 171 + 1.4 59.4 + 0.8 6.0 + 0 0.41 + 0.01 - - - -

Marls Bead S11 F 170 + 2.8 60.6 + l. 9 4.6 + 0.3 - - -

IVS-G 11 F 210 + 2.8 63.4 + 2.4 4.4 + 0 0.46 + 0 - - - -

C = coarse Fract1on F = F1nes Fract1an S = Sequentially class1fied speed

Speed = rev./mln x 1000

Page 100: Durham E-Theses Aspects of structure and functionality in

SPAR3IN3

Co.& /~c F.E. F.V.S. F.L.S. 1CX3 ~~]* C 3min

Cl

6.4 143 68.1 19.7 -0.23 0.33

7.5 150 72.6 26.3 -0.36 0.43

5.4 128 49.1 6.6 -0.65 0.14

6.6 145 64.2 14.9 -0.36 0.29

5.0 138 46.4 14.5 -0.56 0.11

6.7 150 64.2 11.8 -0.39 0.24

6.3 141 62.8 11.8 -0.33 0.22 .

6.3 -0.51 0.15

7.1 -0.91 0.13

4.3 133 24.3 1.3 -0.78 0.05

6.5 128 52.0 7.9 -0.81 0.15

5.6 141 27.3 2.6 -0.70 0.09

5.5 163 57.5 2.6 -0.51 0.17

5.2 140 57.1 5.3 -0.56 0.13

5.2 143 60.5 6.6 -0.57 0.12

5.0 140 56.6 5.3 -0.49 0.13

* t 1s 0 - 0.9 rn1n.

- 82 -

Page 101: Durham E-Theses Aspects of structure and functionality in

Purified llS and 7S prote1ns from bean and pea were tested by

the sparging method only. They had lower initial conductivities than

a-case1n, sodium caseinate, soy whey protein and BSA. However, their

foam stability index was h1gh. They had superior funct1onality

compared to flours, 1solates, proteinates and micellar proteins.

Full-fat flours, isolates, proteinates and micellar prote1ns

gave lower values of F.E., F.V.S., F.L.S. (from whipping experiments),

Cl and CoA/Llc than their equivalent defatted samples. F.E., F.V.S.

and Ci were s1milar for isolates and prote1nates, but Maris Bead had

h1gher values of F.E. and F.V.S. than IVS-G. Soy 1solate was superior

to other isolates, but defatted soy flour had equ1valent functionality

WIth respect to foaming power and foam stability. IVS-G and F1lby

micellar proteins were 1nferior to isolates and proteinates.

With the exception of defatted soy flour, flours had poor

foaming properties. Coarse fractions from air classif1cation

experiments were inferior to fines fractions. Foaming ability of the

fines fractions 1ncreased with classifier speed and protein content of

the fraction.

Foam decay curves of standard proteins are shown in Figure 26.

Both a-casein and BSA had high Initial conductivity and relatively

flat curves. This suggests good foam expansion and stabil1ty.

Myoglobln and lysozyme had steep lnitial slopes indicat1ve of the

brittle foams they produce. The similar foam decay curves produced by

bean and pea llS and 7S proteins (Figure 27) suggest a similarity in

the1r foaming propert1es. The curves are relatively flat wh1ch is

lndicative of good foam stability.

- 83 -

Page 102: Durham E-Theses Aspects of structure and functionality in

2.2 . Figure 26. Foam decay curve&'· of selected protein standards.

2.0

BSA 6.

1.8 a-casein 0

Hemoglobin • 1.6 Myoglobin 0

Oval:>umin .. - 1.4 e c,)

Lysozyme • ' Cl)

e 1.2 ->o .. > ;: 1.0 c,) :::J

CX> ,

-'=" c 0 (.) 0.8

I ~ --- :~ -0.0 • • I i. I Q; I 4

o.o 1.0 2.0 3.o 4:o 5.o 0o 1.0 a.o e.o 10 Time (min)

Page 103: Durham E-Theses Aspects of structure and functionality in

Figure 2 7. Foam decay curves of purified bean and pea proteins. 1.5

Maris Bead 7 S 6.

Maris Bead 11 S 0

IVS-G 11 S • Birte 7 S •

_ 1.0 r\\ \ IVS-G 7 S A E ()

....... 0 E -1: > .. ()

00 :::t .,

U'1 c 0 (,)

0.5

0 0 I I I I I I I I I I I

. 0.0 1.0 2 .. 0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10 Time (min)

Page 104: Durham E-Theses Aspects of structure and functionality in

Foam decay curves of selected soy bean products are sham in

Figure 28. Soy whey protein had superior properties to other products.

The isolate and defatted soy flour had very similar curves, as did the

full-fat soy flour and the soy concentrate.

Foam decay curves of sod1um case1nate, spray dr1ed egg wh1te,

and F1lby pea whey prote1n (F1gure 29) ~ selected flours (Figures 30

and 31), defatted and full-fat 1solates (F1gures 32 and 33), defatted

and full-tat proteinates (Flgures 34 and 35) and defatted micellar

prote1ns (F1gure 36) are shown. Defatted and full-fat soy flour were

shown to be supenor to bean and pea flours. However, bean and pea

1solates produced s1m1lar curves to soy isolate (F1gure 32). Generally

all defatted and full-fat 1solates and proteinates tested were s1m1lar

with respect to 1nit1al conductiv1ty. However, full-fat products

showed a greater 1nitial loss of conduct1v1ty.

M1cellar proteins exh1b1ted greater var1at1on in the1r foam

decay curves. Defatted and full-fat Marls Bead m1cellar prote1ns had

s1milar curves to 1solates and prote1nates. The F11by and IVS--G curves

had lower 1n1t1al conduct1v1t1es and a steeper in1t1al drop 1n

conduct1v1ty. The Marls Bead micellar prote1n used in this exper1ment

was prepared us1ng a d1alyzer/concentrator to reduce the supernatant

volume. The IVS-G and F11by micellar prote1ns had been prepared by the

method of Murray et al. (1978).

The wh1pp1ng and sparg1ng methods were compared, Wlth respect

to foam expansion and foam stab1l1ty, by linear regress1on analysis of

a) all the data points and b) standard proteins. Correlat1on

coefflc1ents are shown 1n Table 17. F.E. determined by the wh1pp1ng

method d1d not correlate strongly with any of the measures of foam1ng

power employed for the sparg1ng method. The best correlation occurred

- 86-

Page 105: Durham E-Theses Aspects of structure and functionality in

CX> ~

-E u (/) e ->­.... > ;: u :I , c: 0

C.)

2.0 Figure 28. Foam decay curves of soy products.

Soy whey isolate • Defatted soy isolate •

1.6 1- \ Defattect soy flour 0

Full-fat soy flour • Soy protein concentrate A

0.0 I I I I I I I I I I 1

0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10 Time (min)

Page 106: Durham E-Theses Aspects of structure and functionality in

co co

-E C)

....... 0 E -""

2.0

1.5

Figure 29. Foam decay curves of sodium caseinate, spray dried egg white and Filby whey protein.

Spray dried egg white Sodium ca.seinate

Filb-y whey protein

• • •

" 1.0 -... C) :J

1 0 (.)

0.5

0.0 I I I I I I I I I I I 0.0 1.0 2.0 3.0 4.0 6.0 6.0 7.0 8.0 9.0 10

Time (mtn)

Page 107: Durham E-Theses Aspects of structure and functionality in

1.2 Figure 30. Foam decay curves of defatted bean and pea flours.

1.0 I \

Defatted soy flour • Defatted Maris Bead flour •

i 0.8 i \ Defatted Filby flour • Defatted IVS-G flour 0

u Us E -~ 0.6 > -.. u

co ~

1.0 '0 c 0

(,)

0.4

0.0 I I I I I I I I I I I

0.0 1.0 2.0 3.0 4.0 5.0 ·6.0 7.0 8.0 9.0 10 Time (min)

Page 108: Durham E-Theses Aspects of structure and functionality in

1.2 Figure 31. Foam decay curves of full-fat bean and pea flours.

1.0 I \

Full-fat soy flour • Full-fat Maris Bead flour .... Full-fat Filby flour • e 0.81 \ . Full-fat IVS-G flour 0

C) ........ U)

E ->-:;: 0.6 ;: CJ ::J

..0 , 0 c

0 (,)

0.4

0.2

I ~ -00 7 I I t;r JF 'tiL 4 - ~· ;' ~ ~ .~ .

· o.o 1.0 2.0 3.o.o.o '::o To 8.0 9.o 10 Time (min)

Page 109: Durham E-Theses Aspects of structure and functionality in

\0 .....

-E u

....... 0 E -~ ~ .. u :t ~ c 0 (.)

1.5

1.0

0.5

Figure 32. Foam decay curves of defatted bean and pea isolates.

Defatted soy isolate •

Defatted Maris Bead isolate 6.

Defatted Progreta isolate •

Defatted IVS-G isolate o

0.0 I I I I I I I I I I I 0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10

Time (min)

Page 110: Durham E-Theses Aspects of structure and functionality in

1.2 Figure 33. Foam decay curves of full-fat bean and pea .isolates.

1.0 W.\ Full-fat Progreta isolate .... Full-fat Maris Bead isolate 6.

Full-fat Filby isolate • Full-fat IVS-G isolate 0

0.8 -e u ' 0 e ->-!: 0.6 > :;:; u

\.0 :I N

, c 0

(.)

0.4

0.2

0.0 I I I I I I I I 0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10

Time (mtn)

Page 111: Durham E-Theses Aspects of structure and functionality in

-e u

....... en e -~ l: .. g

\J:)

! w

1.5

1.0

0.5

Figure 34. Foam decay curves of defatted bean and pea proteinate&.

Defatted Maris Bead proteinate fl.

Defatted Progreta ·proteinate •

Defatted IVS-G proteinate o

Defatted Filby proteinate •

0 0 I I I I I It I I I I I . 0.0 1.0 2.0 3.0 4.00 6.0 7.0 8.0 9.0 10

Time (mtn)

Page 112: Durham E-Theses Aspects of structure and functionality in

1.6 Figure 35. Foam decay curves of full ... fat bean and pea proteinate&.

Full-fat Maris Bead proteinate •

Full-fat Filby proteinate •

1.0 Full-fat IVS-G proteinate • -E Co)

<n E -l: > ;: Co) =t

\,() '0 -'=" c 0 u

0.6

0.0 I I I I I I I I I I I 0.0 1.0 2.0 3.0 4.0 6.0 6.0 7.0 8.0 9.0 10

Time (min)

Page 113: Durham E-Theses Aspects of structure and functionality in

1.5 Figure 36. Foam decay curves of bean and pea micellar proteins.

Defatted Maris Bead micellar protein ~

FuU-fat Maris Bead micellar protein •

Defatted Filby micellar protein 0 1.0 - Defatted IVS-G mice,llar protein o

E (,)

........ Cl)

E ->-.. > ;: (,) :::J

\0 /g V1

0 CJ

0.6

0.0 I I I I I I I I I I J 0.0 1.Q 2.0 ""'"' .. ,. """' A,. _,.. ,..,.. ,..,.. ~

Time (min)

Page 114: Durham E-Theses Aspects of structure and functionality in

TABLE 17. Comparison of whipping and sparging methods for determining foam expansion and foam stability.

CORRELATION COEFFICIENTS

SPARGING

ALL SAMPLES STANDARD PROTEINS

Ci I I log [~~] I Ci I I I

mS em -1 I F.E. I I mS em -1 I I I F.E.

log [~~] F.E. I I I

I I I I I I I I I I I

0.71 I 0.30 I 0.38 I 0.67 I I I 0.39 -0.30 \0 I WHIPPING C7\ I

I I I I I I I I I I I I I

Co • At I AC I F.V.S. I C 3 min I Ci I Co • ~t 1 ~c I I I F.V.S. C 3 min I Ci F.V.S. I I I I

I I I I

I I I I I I I I

0.70 I 0. 73 I 0.70 I 0.95 I I I 0.99 0.88

Page 115: Durham E-Theses Aspects of structure and functionality in

Wlth 1n1t1al conduct1v1ty. However, F.V.S. determ1ned by the wh1pp1ng

method d1d correlate with all three measures of foam stab1l1ty

employed for the sparg1ng method when standard prote1ns were used.

SDS-PAGE of liqu1d dra1ned from a foam of 0.5% defatted Marls

Bead 1solate at selected t1me 1ntervals 1s shown 1n F1gure 37. No

preferent1al retent1on of any prote1n spec1es was observed.

The effect of sugar on the toam1ng ab1l1ty of a 0.5% solution

of defatted Marls Bead prote1nate is shown 1n Table 18. Stirring the

solut1on w1th sucrose pr1or to foaming greatly reduced F.E. and F.V.S.

However, although F.E. and F.V.S. d1d decrease w1th 1ncreas1ng sucrose

content, delay1ng the addit1on of sucrose enabled both F.E. and F.V.S.

to be ma1nta1ned close to their or1g1nal values.

4.6 ASSESSMENT OF EMULSION AcriVITY.

The results of tests on flours, concentrates, 1solates,

prote1nates, m1cellar prote1ns and pur1fied prote1ns to determ1ne

emuls1fy1ng propert1es are shown in Table 19. Marls Bead and IVS-G

1solates and proteinates emulslfied 1nore 011 than flours and a1r

class1f1ed fract1ons, but sl1ghtly less than the soy concentrate and

soy 1solate whlch emuls1f1ed all the ava1lable 011. Defatted products

generally emuls1f1ed less 011 than equ1valent full-fat products.

Emuls1on act1v1ty decreased w1th decreas1ng prote1n content of the a1r

class1f1ed coarse fract1ons, however, prote1n content was not the only

factor 1nvolved as emulsion act1v1ty was not correlated w1th ml Oll/g

prote1n. Pur1f1ed llS and 7S prote1ns emuls1f1ed more 011 than case1n.

- 97 -

Page 116: Durham E-Theses Aspects of structure and functionality in

FIG UR E 37 . SDS-P AGE of drained liquid from a defatt d ar s Bea isola e .

Mr . 1 o-3

92

67

45

35

25

21 18 .5

12.5

1 2 3 5 6

TRA C SA PLE

1 Liquid drained 0 er-2 Liquid drained af er 1 h. 3 Liquid drained af er 30 in . 4 Liquid dra · ned after 15 min. 5 Unfoamed liq id . 6 Total (before f oam ng ) .

- 98 -

Page 117: Durham E-Theses Aspects of structure and functionality in

TABLE 18. The effect of sucrose on the foaming ability of a defatted Maris Bead proteinate.

Time sucrose was added after start of wh1pping

0 MIN 2 MIN 4 MIN

Sucrose F.E. F.V.S. F.L.S. F.E. F.v.s. F.L.S. F.E. F.V.S. F.L.S. %

0 314 80 21 + 2 + 1.4 + 0.6 - - -

6 300 80 20 312 83 19

12 292 80 24 316 78 12

15 156 68 18 +11 + 3 + 3 - - -

24 284 77 12 292 77 12

30 123 60 12 + 33 + 5 + 0 - - -

60 16 24 12 + 0 + 0 + 0 - - -

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Page 118: Durham E-Theses Aspects of structure and functionality in

TABLE 19. Ernulslon act1v1t1es of flours, concentrates, isolates, proteinates, and m1cellar proteins.

Emulslon Actlvity SAMPLE

ml Oll/g sample ml oll/g proteln

Soy concentrate 5.95 + 0.07 9.0 -

Soy isolate - defatted 6.0 + 0 7.1 -Marls Bead flour - defatted 5.2 + 0 16.0 -IVS-G flour - defatted 5.1 + 0 15.4 -Fllby pea flour - defatted 4.2 0 + 19.4 -IVS-G flour - full-fat 4.8 + 0.7 15.0

-Marls Bead flour - full-fat 4.6 + 0.8 14.4

-Filby pea flour - full-fat 5.3 0.3 23.8 + -

AIR CLASSIFIED FRACI'IONS

MarlS Bead 3 F 5.2 + 0 17.4 -7 F 2.8 + 0.07 4.8 -11 F 4.1 + 0 5.5 -3 c 0.2 + 0 2.9

-5 c 5.3 + 0 23.8 -6.5 c 3.0 + 1.3 17.8 -9 c 4.9 + 0 22.5 -

IVS-G 3 F 5.4 + 0 14.6 -II 5 F 5.4 + 0 13.1 -II 7 F 5.8 + 0 8.8

-II 9 F 5.0 + 0 7.1 -II 3 c 4.4 + 0 27.7

-II 6.5 c 4.1 + 1.3 10.2

-

SOOUENTIAILY CLASSIFIED FRAcriONS

MarlS Bead 9 F 4.1 + 0.4 5.9 -7 F 3.3 + 1.5 5.2 -5 F 3.7 + 1.1 16.5 -

11 c 3.5 + 0.4 16.2 -

9 c 2.3 + 0.4 11.9 -7 c 1.7 + 0.8 11.9 -5 c 0.8 + 0 5.1 -3 c 0.2 + 0 2.9 -

-

F = Fines Fraction c = coarse fraction Speed = rev./min x 1000

Page 119: Durham E-Theses Aspects of structure and functionality in

--

Emulsion Act1v1ty SAMPLE

ml ml/g sample ml ml/g prote1n

SEQUENTIALLY CLASSIFIED FRACI'IONS

IVS-G 11 F 5.5 + 0.1 7.4 -II 9 F 5.5 + 0.1 7.7 -II 7 F 5.4 + 0.5 12.2 -II 5 F 2.9 + 0.1 21.8 -II 3 F 4.3 + 1.1 17.6 -II 11 c 3.9 + 0.6 19.6 -II 9 c 4.0 + 0 21.2 -II 7 c 2.8 + 0.3 17.6 -II 5 c 2.4 + 0.5 14.9 -II 3 c 0.2 + 0 2.2 -

--·- -- -

MB proteinate - full-fat 5.8 + 0 7.0 -IVS-G proteinate - full-fat 5.95 + 0 6.6 -MB proteinate - defatted 5.6 + 0.4 6.2 -MB 1solate - full-tat 5.7 + 0 6.3 -IVS-G 1solate - full-fat 5.8 + 0.3 6.2 -Progreta 1solate - full-fat 4.3 + 0.1 5.1 -MB 1solate - defatted 5.6 + 0 5.9 -MB m1cellar proteln-full-fat 5.0 + - 0 5.0 MB m1cellar prote1n-defatted 5.6 + 0 5.6 -

PROI'EINS 0.1 g/10 ml

Marls Bead 11 s 29.5 + 0 -

IVS-G 11 s 25.0 + 0 -Maris Bead 7 s 23.8 + 3.2 -IVS-G 7 s 24.0 + 0

-Case1n 1.8 + 1.5 Case1n 0.5 g/10 ml 5.5

-+ 0 -

- - --

F = F1nes Fract1on c = coarse fract1on Speed = rev./m1n x 1000

MB = Marls Bead

All results were the average of at least two tests. Micellar prote1ns were prepared by ultraf1ltrat1on.

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4. 7 DIFFERENTIAL SCANNING CAI.DRIMETRY.

A differential scann1ng thermogram of Maris Bead flour 1s

shown in Figure 38. There were two maJor transitions and a third lying

between them. The isolates, proteinates and micellar proteins d1d not

have the first low temperature transition, therefore this was

attr1buted to starch gelatinization. The other two peaks were assigned

to legumin and vicilin after comparison with the Tm and Tmax values of

the pur1f1ed proteins. Purified llS and 7S proteins produced only one

peak. Transition temperatures of flours, isolates, proteinates,

m1cellar proteins and purif1ed proteins are shown in Table 20. Peaks 2

and 3 from Maris Bead flour had h1gher Trnax values than equivalent

peaks from 1solates, proteinates and m1cellar proteins. Average Tmax

values for the latter were 361.9 ~ 0.74 K and 369.8 ~ 0.74 K for peaks

2 and 3 respectively. Purif1ed llS and 7S proteins had the lowest Tmax

values, 368.4 K and 357.4 K respectively. There were fewer values of

Tm or Tmax recorded for peak 2 as the shape of the peak made

determination of these values difficult.

~H values for denaturation of the samples varied with the type

of sample. Proteinates had the lowest~ values (3.34 ~ 0.53 cal g-')

and m1cellar proteins the highest (5.00 cal g-' for flocculated

samples and 4.54 for the sample prepared with the

d1alyzer/concentrator); 1solates had intermed1ate values (3.91 + 0.05

cal g-' ). Aging the proteinate sample for two years was shown to

shghtly reduce ~. The proportion of total protein represented by

legumin in flours, 1solates, proteinates and micellar proteins was

66.0 + 3.9%, where total prote1n 1s defined as legumin plus v1c1l1n

only, and ~ values of 5.4 _, _,

cal g and 4. 6 cal g were used for

legum1n and v1cilin respectively (Wright and Boulter, 1980).

- 101 - ~·( 0 ll,v t~

z.

Page 121: Durham E-Theses Aspects of structure and functionality in

~

0 1'\)

i .s • G 2:

i 'I ! • ;: a

320

Figure 38. DSC thermogram of M~rta Bead flour.

STARCH

340 360

Temperature (K)

VICILIN LEGUMIN

380 400

Page 122: Durham E-Theses Aspects of structure and functionality in

TABLE 20. Trans1t1on temperatures ot Marls Bead and IVS-G flours, 1solates, prote1nates, m1cellar proteins and pur1fied proteins.

1 2 3

SAMPLE Tm T max Tm T max Tm T max (K) (K) (K) (K) (K) (K)

--Marls Bead flour 330.4 337.7 364.3 374.0

+0.3 +0.2 +0.3 - - -

Marls Bead proteinate 369.5 +0.3 -

Marls Bead prote1nate 361.5 369.8 aged 2 years +1.0 +0.32 - -

IVS-G prote1nate 361.9 368.8 1983 sample +0.2 +0.3

- -

IVS-G proteinate 368.7 1985 sample +0.32 -

Marls Bead isolate 370.0 +0.9 -

IVS-G isolate 363.0 370.2 +0.4 +0.5 - -

Marls Bead m1cellar 370.6 prote1n U/F +0.2

-

Marls Bead micellar 361.0 370.9 protein ( diluted ) +0.6 +0.3

- -

IVS-G m1cellar prote1n 362.1 369.8 ( d1luted ) +0.8 +0.4

- -

MarlS Bead llS 360.8 368.9 +0.6 +0.3 - -

IVS-G llS 360.5 367.9 +1.1 +l.l - -

Marls Bead 7S 347.8 355.8 +0.9 +0.6 - -

IVS-G 7S 349.8 359.0 +0.2 +0.2 - -

--All the temperatures are the average of s1x samples. U/F = Prepared by ultraf1ltrat1on.

- 103 -

AH

Cal g"'"1

2.98 +0.2 -

2.80 +0.1 -

3.76 +0.2 -

3.83 +0.3 -

3.55 +0.1 -

4.26 +0.3 -

4.54 +0.1 -

5.09 +0.3 -

4.92 +0.3 -

5.02 +0.4 -

5.43 +0.4 -

4.83 +0.3 -

5.64 +0.2 -

Page 123: Durham E-Theses Aspects of structure and functionality in

rnAPI'ER 5

DISOJSSICN

Leguminous seeds contain a number of constituents which are of

potential interest to the food manufacturing Industry, ie. oil,

protein, starch and fibre. Available technology can be used to produce

a range of products with varying physical and chemical properties in

an attempt to meet the requirements of the food processing industry.

In this thesis a number of processing methods were used, and the

samples were assessed for functionality in some model tests.

Flours.

Prote1n contents of Marls Bead and IVs-G flours were

approximately 32% on a dry weight basis (Table 1). This compares with

prev1ously reported values for Marls Bead of 32.8% and 34.7% (Bhatty,

1974). Generally spring sown var1et1es of V1c1a faba m1nor, such as

Marls Bead, have prote1n contents rang1ng from 25.5 35.4%, and

winter sawn var1eties have sl1ghtly lower protein contents, ranging

from 24.3- 29.9% {Eden, 1968). These values also include free arn1no

acids wh1ch may account for 0.73-1.5% of the flour and cons1st chiefly

of arg1nine residues (Barratt, 1982). Var1et1es with a h1gh protein

content also have hlgh levels of free amino ac1ds. Eden { 1968)

reported true protein levels of 22.3 31.7% in 104 spr1ng sawn

- 104 -

Page 124: Durham E-Theses Aspects of structure and functionality in

varieties. Th1s compares with typical values for crude protein of 22%

and 40% for peas and soy beans respectively.

The starch content of IVS-G flour was 7% lower than that of

Maris Bead (Table l). Bhatty (1974) reported starch contents of 35.0

and 37.8% on a dry weight basis for Marls Bead. These values are lower

than those found in the present study. However, he did report slightly

higher values for protein content for Maris Bead, and protein and

starch contents have been shown to be inversely correlated (Bhatty,

1974; Barratt, 1982). Starch contents of 28- 40% and 35 53% were

reported for a nwnber of varieties of tield beans by Bhatty (1974) and

Barratt (1982) respectively. Typical starch contents of peas and soy

beans are 47% and 0 respectively.

A comprehensive analysis of field bean composition was

conducted by Eden ( 1968) , and field bean carbohydrates were discussed

by Pritchard et al. (1973).

The composition and potential uses of full-fat soy flour have

been discussed by Pringle (1974). Generally full-fat products have

limited market potent1al because of poor functionality and storage

problems assoc1ated with high lip1d contents (Wolf, 1975; St. Angelo

and Ory, 1975; St. Angelo and Graves, 1986). This is particularly

relevant to 011 seeds, which store 011 in preference to starch, eg.

soy and peanut. Soy beans have a lipid content of 22%, compared to

1-2% 1n f1eld bean (Eden, 1968).

Defatting the flours marginally Increased their protein

contents to approximately 33% (Table 1). Defatted soy flours typically

have a prote1n content of 56%. Extraction of l1pids with hexane only

removes the non-polar l1p1ds. In pea this accounts for only 40% of the

total lipld (Wright and Bumstead, 1984). The remaining fraction

- 105 -

Page 125: Durham E-Theses Aspects of structure and functionality in

oons1sts primar1ly of polar phospholipids and glycolip1ds which can be

renoved by subsequent extraction in var1ous solvent systems. Hc:J,o~ever,

this usually results in a loss of solubility (Wu and Inglett, 1974).

Eldridge et al. {1971) showed that a mixture of 20% hexane and 80%

2-propanol caused the least subsequent insolubilization of soy bean

flours. Defatted soy flours and grits form the largest part of the

market for soy products in the United States, and a wide range of

products differing in composition and physical properties are

commercially available (Kellor, 1974).

Production of Protein and Starch Concentrates.

The technology developed for the processing of soy beans can

be successfully applied to grain legume crops. The processes involved

are summarized 1n Figure 39 (Wright and Bumstead, 1984). Hc:J,o~ever, an

alternative method is available for the production of high protein and

high starch fractions from legumes; namely air class1ficat1on. The

basis of separation is the internal composition and organization of

cereal and grain seeds. In legumes storage proteins are located in

d1screte protein bodies with a diameter of approximately 3 ~m (Weber

and Neumann, 1980). Protein bodies of VIcia faba cotyledons have been

studied by Briarty et al. {1969), and compared to those of pea

cotyledons by Weber et al. {1981). The starch is located In much

larger granules, ranging in size from 25-40 ~m (Vose et al., 1976).

Early reports suggested that legumes conta1ned a single population of

starch granules (B1l1aderis et al., 1981). However, more recent

ev1dence suggests that some legumes conta1n significant populat1ons of

starch granules w1th a diameter of less than 10~m (Ring, 1983). The

s1ze differential between protein and starch constituents facilitates

their separation dur1ng air classlfication to yield protein and starch

- 106-

Page 126: Durham E-Theses Aspects of structure and functionality in

Figure 39. Processing of soy beans.

Soy beans

de-hulling --------------~ hulls

flaking

Full-fat flour

solvent l extraction

Defatted flour __________ ! ________ __

(I) aqueous alcol:lol wash

(ii) acid leach

(IIi) moist heat, water wash

enriched fractions.

Soy Protein Concentrate

aqueous extraction

centrifuge

adjust to pH 4.5

Soy Isolate

~ neutralize

Soy Proteinate

Prior to air classification the seeds are split and milled.

For the air classification process to be efficient the milling process

must effectively separate the flour into its constituent particles,

ie. starch granules and protein bodies.

It was noted that IVS-G seeds took longer to split on the

end-runner m1ll than those of Maris Bead. Therefore, it is likely that

seeds of IVS-G are harder than those of Maris Bead. Seed hardness, as

measured by grinding time, was shown to be negatively correlated with

- 107 -

Page 127: Durham E-Theses Aspects of structure and functionality in

IOC)isture content for field peas and faba beans by Tyler and Panchuk

(1982). However, KoslOC)lak (1978) and Obuchowski and Bushuk (1980)

reported longer gr1nd1ng times for softer cultivars of wheat, and for

a single cultivar as moisture content was increased. This probably

reflects d1fterences in internal structures between cereals and grain

legumes. The observed d1fferences in grinding time between Maris Bead

and IVS-G seeds could not be attributed to differences 1n moisture

content (Table 1), so must reflect a genuine difference in structure

between the seeds.

Moisture contents of the flours were 11 11.5%. This is

h1gher than the opt1mum values reported for air classification by

Tyler and Panchuk (1982). They classified samples of field peas and

taba beans w1th mo1sture contents ranging from 3.8 - 14.3%. Seed

moisture contents of greater than 9% significantly affected both yield

and oompos1t1on of the air classifled fractions. Seeds w1th low

mo1sture contents produced fract1ons with decreased starch fraction

y1eld, protein content of the starch and protein fractions and starch

separat1on effic1ency (SSE), and increased protein fraction y1eld,

starch content of the coarse and fines fractions and prote1n

separat1on efficiency (PSE). This was attr1buted to more eff1c1ent

part1cle size reduction during milling in seeds with a low moisture

content. During pin mill1ng seeds are shattered as they strike a hard

surface at speed. More brittle seeds would presumably undergo a

greater particle size reduction. The increased starch content of the

f1nes fraction was probably due to starch damage during the milling

process, although an 1ncreased proportion of damaged starch granules

was not detected by the1r assay.

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Page 128: Durham E-Theses Aspects of structure and functionality in

The coarse fractions obta1ned from Ivs-G tlour below a

classifler speed of 7000 rev./min were signiflcantly larger than those

obta1ned from Marls Bead (Table 2). PSE was also oomparatively low

(Table 5). Th1s suggests that the p1n milling process was less

effic1ent for Ivs-G seeds, and is contrary to expectat1ons as Ivs-G

seeds appeared to be harder than those of Maris Bead. An efficient

separation 1s dependent on complete cellular disruption during

milling, caus1ng a release of protein and starch storage organelles as

separate ent1ties. Differences 1n impact milling efficiency may result

from differences in a) the am:::>unt of cell wall matenal (CWM), b) the

th1ckness and structural rigidity of the cell wall, c) the degree of

adhes1on between the cell contents and the cell wall, d) the degree of

adhesion between prote1naceous material and starch granules, e) the

extent to whlch prote1naceous mater1al 1s broken into unit part1cles,

and t) the degree of adhes1on between indiVldual cells (Tyler, 1984).

An 1ncrease 1n any of the above characteristics would cause an

increase in the energy input requued to achieve <X>Illplete cellular

disrupt1on.

After a second pass through the p1n mill the Ivs-G coarse

fract1on was s1gn1f1cantly reduced at all classifier speeds (Table

2a), and there was a concom1tant decrease in the prote1n oontent of

the f1nes fract1on and increase 1n PSE (Tables 3a and Sa

respectlvely). Protein content of the fines fraction presumably

decreased due to the concentrat1on of other cellular components in the

fines fraction, eg. starch and CWM (Tyler and Panchuk, 1982). A hlgh

proport1on of starch was found m the fines fract1on and SSE was la.v

at 6500 and 7000 rev./m1n compared to values obta1ned for Maris Bead

(Tables 4 and 6). Thls may have been attnbutable to starch damage

dur1ng the second m1ll1ng step.

- 109 -

Page 129: Durham E-Theses Aspects of structure and functionality in

A number of studies have shown that repeated milling steps

reduce the protein content of the starch fraction (Vose et al., 1976; --Reichert and Youngs, 1978; Tyler et al., 1981; Tyler, 1984; Wright et

al., 1984). The latter authors observed that repeated milling prcxiuced

an increased proportion of particles with a diameter of less than 20

~m, largely at the expense of particles in the 25-30 ~m d1ameter

range. The latter were assumed to be protein body agglomerates and

starch-protein body agglomerates. These have been observed using SEM

(Reichert and Youngs, 1978). However, total separation of starch and

protein components is not easy to achieve as a proportion of the total

protein remains attached to the starch granules despite four or five

m1lling steps. After five mill1ng steps northern beans, field peas and

oowpeas had coarse fractions w1th protein contents of 3.1, 2.7 and

3.3% respectively (Tyler, 1984). Colonna et al. (1980) reported coarse

fractions w1th 2% protein from faba beans and smooth seeded peas after

two and three mill1ng steps respect1vely. This residual prote1n has

been shown by SEM to consist of starch granules embedded in a protein

matrix (Reichert and Youngs, 1978). After milling and a1r

class1f1cat1on of peas which retained their green colour at maturity

the agglomerates were shown to be chiefly composed of starch granules

and chloroplast remnants. The adherent protein can be explamed by

cons1derat1on of the physiology of the develop1ng and mature pea

cotyledon (Ba1n and Mercer, 1966). From 10 20 days after

fert1l1zation a s1ngle starch granule 1s init1ated in most pea

chloroplasts in the embryo. The starch granule graws rapidly from days

20 45, disrupt1ng the structure of the plastid and compressing the

lamellae and grana aga1nst the limiting membrane of the chloroplast.

Me.':lbrane remnants pers1st around the starch granules in the mature pea

cotyledon. Slmilarly, Barlow et al. (1973) have demonstrated the

ex1stence of membrane remnants surrounding starch granules in wheat.

- 110 -

Page 130: Durham E-Theses Aspects of structure and functionality in

It is possible to obta1n almost pure starch fractions by

repeated water washings to remove the res1dual protein. Vose et al.

{1976) obtained starch fract1ons with 0.15 and 0.05% nitrogen from

horse beans and field peas respectively. The isolation of pure starch

by conventional wet process1ng methods is also difficult due to the

presence of a highly hydrated fine fibre fraction, probably derived

from the cell wall (Vose et al., 1976).

However, there are d1sadvantages in using repeated milling

steps. As mentioned previously the protein content of the fines

fraction tends to decrease with successive milling steps. This is

accompanied by an increase in starch content, attributable to damage

of starch granules dur1ng m1ll1ng (Vose, 1977; Reichert and Youngs,

1978). Vose {1977) observed that the proportions of starch granules

suscept1ble to enzymic hydrolysis were 21.8, 5.8 and 23.9% after two

mill1ng steps, and 39.6, 8.8 and 32.6% atter four milling steps for

pea, corn and wheat starches respectlvely. SEM demonstrated that some

starch granules had been shattered whilst others had superficial

exfoliation of the surface. Reclassification of the flour results in

some of this starch being classif1ed into the f1nes fract1on, causing

a decreased protein content 1n the fines fract1on and SSE, and an

increased starch content of the fines fract1on.

Damaged starch granules were shown to exhibit increased

V1scos1ty dur1ng pasting compared to native starch granules.

At 3000 and 4000 rev./mln the maJor component of the coarse

fract1ons from both Marls Bead and IVS-G was visibly hull material.

This was reflected in the low protein and starch contents of these

fractions {Tables 3 and 4). Wr1ght et al. {1984) observed that at 3000

rev./min the coarse fraction from pea had a high cellulose,

- 111 -

Page 131: Durham E-Theses Aspects of structure and functionality in

hemicellulose and ,PeCtin content. Furtherrrore, the balance of sugars

1n this fraction was similar to that of isolated hull material. Hull

material has been shown to account for approximately 13% of seed

weight in various cultivars of Vicia faba (Griffiths, 1981). Partition

of hull material into the coarse fraction has also been observed by

Vose et al. (1976), Kon et al. (1977), and Sosulski and Youngs (1979).

It is apparent that pin m1lling is not an effective method for

grinding the testa.

Hull material from peas has found a commercial outlet as a

fibre supplement 1n white bread. It has a significantly higher fibre

content (75%) than wheat bran (46%), (Wright et al., 1984). A s1m1lar

use of V1cia faba hulls may be limited by the significant quantities

of tannins that have been reported for some varieties (Gnffiths and

Jones, 1977; Martin-Tanguy et al.~ 1977; Moseley and Gr1ff1ths, 1979).

Tann1n content has been positively correlated with coloured flowers in

Vicia var1et1es (Griffiths, · 1981), and ~lth seed coat colour in

Phaseolus beans (Elias et al., 1979). Maris Bead and IVS~ flowers are

off-white in colour with some darker petal markings. Furthermore,

Marls Bead seeds are dark brown in colour. IVS~ seeds vary in colour

from light green to buff. It is probable that both contain significant

tann1n levels, although IVS~ may have lower levels than Marls Bead.

Tannins have been shown to a) have an astringent taste, b) adversely

affect protein solubility, and c) to inhibit digestive enzymes

including tryps1n, a-amylase and l1pase (Griffiths and Jones, 1977;

Griffiths, 1979). Whether these properties are significant at the

appropriate inclusion rates for hull materials into processed foods

needs further investigation. The use of white seeded or white

flowering types would circumvent these problems.

- 112 -

Page 132: Durham E-Theses Aspects of structure and functionality in

Hull material does not contribute to the ftu1ct1onal or

nutr1tional properties of

has been shown to improve

flours or protein concentrates. Dehulling

the funct1onal properties of Phaseolus

vulgaris flours (Deshpande et al., 1982), and the nutrit1onal

properties of Vicia faba flours when fed to animals (Nitsan, 1971;

Marquardt and campbell, 1973; Martin-Tanguy et al., 1977; Moseley and

Grlffiths, 1979; Fowler, 1980).

Air classiflcation of Maris Bead and twice-milled Ivs-G flours

generally gave sim1lar results, w1th the exception of at 3000 rev./min

where IVS-G flour produced a significantly larger coarse fraction

(Table 2). Th1s could be attributed to less efficient size reduction

of e1ther hull material or starch protein agglomerates. Air

class1f1cat1on results for Maris Bead and twice-m1lled IVS-G flours

were compared with those of Wright et al. (1984) for the air

classificat1on of Filby pea flour performed under s1milar oondit1ons.

The maJor d1fferences observed were as follows:

1) at 3000 rev./min the coarse fractions of Marls Bead and

IVS-G were larger. Th1s can be attnbuted to a larger pro:p:>rtion of

hull mater1al in the Vic1a faba beans. Gnfhths (1981) re:p:>rted hull

contents of 8.2 and 13% for Filby pea and Vicia faba var1et1es

respectively.

2) from 4000 - 6500 rev./min F1lby pea produced larger yields

of coarse fract1on, attributable to the higher starch content of peas.

3) protein percentages were higher in both coarse and fines

fract1ons for Maris Bead and IVS-G, reflect1ng the h1gher 1n1tial

prote1n content. The h1gher prote1n content of the coarse fract1on was

presumably due to protein body agglomerates and starch-prote1n body

agglomerates.

- 113 -

Page 133: Durham E-Theses Aspects of structure and functionality in

4) Starch percentages were h1gher 1n both coarse and fines

fractions for Filby pea. This was attributed to its higher initial

starch content. The higher starch content of the fines fraction was

probably due to either a population of small starch granules or a

larger number of damaged starch granules.

5) PSE was higher for Maris Bead and IVS-G flour. The higher

starch content of Filby flour would result in an increased proportion

of protein of chloroplast origin associated w1th the starch granules.

Th1s prote1n is more difficult to separate during milling.

6) SSE was higher for Filby pea flour.

The highest starch and lowest protein conta1ning fractions for

both Maris Bead and IVS-G seeds were obtained in the coarse fractwn

produced at 6500 rev./min. Th1s corresponds to a cut point of 18.5 ~m.

Wright et al. (1984} analysed particle size distributions of a) pea

flour produced by a single pass through a Kolloplex mill, b) pure pea

starch, and c) fines and coarse fractions obtained by air

classiflcation, us1ng a Coulter counter. They found 90% of part1cles

had a d1ameter of less than 40 ~m in the milled flour. The peak for

pure starch was at 22 ~m, and a peak in the whole flour was observed

at 22.5 ~m. Analys1s of the coarse and fines fractions showed that cut

po1nt was not sharply defined during air classification. However,

plotting cut point aga1nst fines fract1on yield does give some

1nformat1on on particle size distr1bution (F1gure 2). 82 and 74% of

Marls Bead and IVS-G particles respectively had a diameter of less

than 40 ~m. There was a bulge in the graphs showing a large proportion

of part1cles between the cut po1nts of 16 and 24 ~m. Coarse fractions

obta1ned between these cut points had the highest starch contents,

ind1cat1ng that the bulk of the starch granule populat1on occurs 1n

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this region (F1gures 3 and 4). Protein content of the fines fraction

declined steeply between 10 and 16 p,m, indicating that rrost

proteinaceous material had a particle diameter of less than 10 p,m.

Individual protein bcXiies have a diameter of approximately 3 p,m (Weber

and Neumann, 1980). However, protein bcXiy agglomerates would be of a

greater size. Peaks corresponding to particle sizes of 2,4,7 and 11 p,m

were observed in whole pea flour by Wright et al. (1984). These were

all attributed to prote1n body agglomerates. In the sequent1al

classif1cat1on exper1ment 14% of the flour had a particle diameter

< 10 p,m, and this fraction had a prote1n content of 75% (Table 8,

Figure 6). Relat1vely small quant1t1es of flour were obtained between

the cut po1nts of 10 and 18 p,m. These fract1ons also had a h1gh

protein content and presumably consisted largely of protein body

aggregates. Fines fract1on size increased dramatically between cut

points of 18 and 30 p,m, and was accompanied by an equally dramatic

fall In protein content. This is largely attributable to the

fractionation of starch granules into the fines fraction. At a cut

po1nt of 40 p,m the coarse fraction was composed predominantly of hull

material.

A single m1lling and a1r class1fication yielded flours with up

to 75% prote1n. However, this accounted for only 29 and 36% of the

total protein 1n IVS-G and Marls Bead flours respect1vely. Comparative

figures for Filby pea were 55% protein accounting for 29% of the total

protein (Wright et al., 1984). Conventionally protein concentrates

produced by the a1r class1fication method undergo an initial milling

and air classlfication step, followed by remilling and classifying the

coarse fraction. The two f1nes fractions are combined to g1ve the

prote1n concentrate. This results In a large yield of high protein

product. The coarse fraction obta1ned at 6500 rev./min was used for

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the reclass1flcat1on expenment as 1t had the highest starch content,

and the corresponding fines fraction had a reasonable y1eld and

prote1n content (Tables 2,3 and 4).

The 1nitial classificat1on at 6500 rev./man of the

reclassif1cat1on exper1ment produced a PSE value s1gnificantly lower

than in the previous expenment (Table 5; Figure 5). However, at 7000

rev.jm1n in the or1ginal exper1ment PSE was s1m1lar to that obtained

at 6500 rev./min in the reclassif1cat1on exper1ment. The difference 1n

cut .Pcnnt obtained at these two classifler speeds 1s very small, and

so the results are not that surprising. Air classification does not

produce a sharply defined cut po1nt, and furthermore, the starch

granule s1ze peak ( 22 f1;n) 1s very close to the cut pmnt used ( 19 p.m) •

A small change in operat1ng cond1tions could result 1n a d1fferent

proport1on of the starch granule papulat1on being classified 1nto the

f1nes fract1on.

Rem1ll1ng the coarse fract1on shifted some of the

prote1naceous mater1al, presumably present as agglomerates of protein

bodies or starch - prote1n bod1es into the f1nes fraction. The three

re-classlf1cat1on speeds used represent cut pomts of 18.5 - 22 p.m,

and were selected as they produce relat1vely large fines fract1ons

w1th h1gh prote1n contents. The small d1fferences observed in the

concentrate y1elds and compositions reflects the small differences 1n

cut point used, and the proxima ty of these cut points to the peak 1n

starch granule size (Table 7). Relat1vely few starch granules were

sh1fted 1nto the fines fract1on even at the lowest class1f1er speed

used. However, prote1n concentrates had a starch content of

approx1mately 20%. A number of factors may have been res_pJns1ble for

th1s. They are: a) the overlap 1n particle s1ze distributions obta1ned

1n the coarse and fines fract1ons by air class1f1cation (Wr1ght et

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al., 1984), b) a population of smaller starch granules (Ring, 1983),

and c) a proportion of starch granules wh1ch sustained damage during

the milling process (Vose, 1977). It should prove poss1ble to reduce

th1s starch content by reducing the cut point used. However, this w1ll

have a detr1mental effect an the fraction yield.

Wright et al. (1984) prcxiuced protein concentrates fran pea

after three milling and air class1fication steps with yields of 35.1

and 26.6%, prote1n contents of 49.5 and 54.1%, and residual starch

contents of 8.1 and 3.9% at 9000 and 11000 rev./ffiln respectively.

Starch concentrates Wlth y1elds of 64.9 and 74.3%, starch contents of

65.4 and 61.3% and residual prote1n contents of 7.1 and 10.2% were

prcxiuced at 9000 and 11000 rev ./mln respect1vely. The lower yield of

prote1n concentrate Wlth equ1valent prote1n content reflects the lower

protein content of the pea compared to faba beans. The higher yields

of prote1n concentrate from bean flours should make their prcxiuction

more of a commerc1al viabil1ty, prov1d1ng they have des1rable

funct1onal and flavour characteristics.

The y1elds of starch and protein concentrates are sl1ghtly

higher and lower respect1vely than those obtained for horse beans by

Vose et al. (1976) using different operat1ng cond1tions. They also

achieved higher starch (69%) and protein (61%) contents in their

starch and prote1n concentrates respect1vely, and lower amounts of

res1dual protein ( 5%)- and contaminating starch ( 11%) . Tyler et al.

(1981) prcxiuced a lower yield (37%) of protein concentrate with a

higher protein content ( 70%) and low starch content ( 4%) from V1c1a

faba minor cv. Diana. They also prcxiuced a starch concentrate

conta1n1ng 81% starch, and only 8% prote1n.

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A number of factors contr1bute 1n determ1n1ng the y1eld and

c~posit1on of starch and prote1n concentrates. They are:

a} In1t1al prote1n content. Generally h1gher y1elds and

prote1n contents of prote1n concentrate are obtained from beans with a

h1gher prote1n content. However, V1c1a faba minor cv. D1ana and V1c1a

faba equ1na L. had sim1lar and lower prote1n contents respect1vely

compared to Marls Bead and IVS-G seeds.

b) Mo1sture content. Both of the above stud1es used flour

equ1llbrated to a mo1sture content of 8%. Th1s may have 1Inproved·

1mpact mllllng effic1ency {Tyler and Panchuk, 1982}.

c) Mllllng procedure. Both of the other expenments used an

Alp1ne Contraplex 250 CW p1n m1ll. Wr1ght et al. (1984) observed that

a greater y1eld of f1nes fract1on: and a h1gher prote1n recovery 1n

the f1nes fract1on were obta1ned dur1ng a1r class1f1cat1on of F11by

pea flour when the Contraplex mill was used Instead of the m1ll

employed 1n this study. Partlcle s1ze reduct1on was probably more

efficient dur1ng mill1ng 1n the other two stud1es.

d) Type of air class1f1er used.

e) Differences In 1mpact mill1ng efficiency,

and f) d1fterences In starch granule s1ze d1str1bution.

Further experiments are needed to 1nvest1gate the poss1bil1ty

ot 1ncreasing the purity of starch and prote1n concentrates w1thout

slgnificantly comprom1s1ng yields, by optimlzing the operatlng

condltions. A change In the milling procedure would probably have the

most signiflcant effect on the y1elds and compos1t1ons of the

concentrates.

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Protein concentrates have been prepared commercially in Canada

from navy beans and field peas, and compete with imported soy products

(Relchert, 1982). Soy protein concentrates typically have a protein

content of 72%. Their composition, nutritional, functional and quality

characteristics have been assessed by Matti! (1974). The prote1n

concentrates produced in this study are more equivalent in protein

content to a defatted soy flour (56% protein). However, ultimately

their use w1ll depend on functional and organoleptic propert1es.

Starch concentrates have found applications in potash ore

refining, as adhesives for corrugated board production, and as

pressure sensitive m1crocapsule coatings for carbonless paper

(Reichert, 1982), as well as applications in the food industry

(Luallen, 1985).

Protein yield (PY) from all of the a1r classificat1on

experiments was generally less than 100% (Table 5). PY was lowest at

h1gh class1fier speeds, where the fines fractions were small. Total

protein recovery is not achieved in practice as very fine particles

are carried through to the air filter by the classifying air stream

(Wright et al., 1984). Values of PY may have been higher for IVS-G as

particle size reduction was less efficient, resulting in fewer very

f1ne part1cles. Values for starch yield (SY) were generally hlgher

than those for PY. However, at 3000 rev./min low values of SY were

obtained. This was attributed to sampling difficulties due to the

heterogeneous nature of the coarse fraction.

Alr classification has considerable advantages over the more

convent1onal wet process1ng methods originally developed for the

production of soy flours, prote1n concentrates and isolates (F1gure

39). Damage to protein constituents may occur at several stages dur1ng

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wet processing, eg. during. solvent extraction, desolventizing or

removal of soluble sugars. The effects of protein denaturation on

funct1onality have been reviewed by Wu and Inglett (1974). The process

is also comparatively expensive as energy input is required to dry the

product after solvent extract1on, sugar removal or isolate product1on,

and effluent has to be disposed of. Furthermore, the activity of

lipox1dases during process1ng may lead to the rap1d development of

rancid and painty odours or flavours (Kon et al., 1970). Heat1ng the

sample to control l1pox1dase act1vity can result 1n further

denaturat1on and loss of functionality. In contrast dry process1ng, by

mill1ng and a1r classification, leaves the prote1n in its nat1ve state

ins1de the protein body. Such protein might be expected to have

superior functional characteristics.

Hcwever, there are some · problems associated w1 th the air

class1f1cation process. Re1chert (1982) showed that the composition of

a1r classified fractions was dependent on the initial protein content

of the flour. For var1et1es which show signlficant variations in

protein content it may prove difflcult to produce concentrates with

cons1stent starch and prote1n contents. A uniform product is of

obvious importance to the food manufacturer. Also, as environmental

factors affect the compositions of lndividual crops it may prove

necessary to optim1ze process1ng conditions for each batch. Th1s would

be expensive 1n time and operator costs. For leguminous crops with low

protein contents it may prove impossible to produce adequate y1elds of

protein fractions with a sufficiently h1gh protein content for

commercial applications. However, starch concentrates produced from

such crops would tend to be large and have low protein contents. The

development of markets for the utilization of starch concentrates may

prove 1mportant 1f leguminous grain crops are to compete w1th the oil

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bearing seeds. The use of starch as a functional ingredient for the

tcx:xi Industry has been recently reviewed by Luallen ( 1985). Its maJor

uses are as thickeners, a source of carbohydrate, stabilizers,

texturizers, water or fat binders, and emulsification aids.

Not all legume flours are suited to the air classification

technique. Starchy legumes. with high llpid contents are not

effectively separated as the lipid causes the flour to agglomerate,

eg. chickpea flour (Sosulski and Youngs, 1979). Also, the technique

has no practical application for oil bearing seeds which have no

differential particle size distribution, eg. soy beans (Ireland et

al., 1986).

Various seed components have been shown to fractionate with

the protein Into the fines fraction. The most significant of these IS

the partition of lipid (Vose et al., 1976; Kon et al., 1977; Sosulski

and Youngs, 1979; Tyler et al., 1981; Wnght et al., 1984). Protein

bodies of au-dned peas have been sha.vn to be coated with a llpid

rich structure (Swift and Buttrose, 1973). Lipid contents of up to 7%

have been reported In pea protein concentrates. Problems associated

with high lipid contents are discussed In the next section. Sugars

also tend to fractionate Into the fines fraction. These Include

sucrose, raffinose, stachyose, galactose, and arabinose (Kon et al.,

1977; Wright et al., 1984). The latter two are associated With cell

walls. Raffinose and stachyose have been implicated as contrlbuting to

flatulence (Wagner et al., 1977). MacArthur and D'Appolon1a (1976)

have shown a slmilar fract1onat1on of sugars during air class1f1cat1on

of wheat. Other components known to fract1onate 1nto the fines

tract1on 1nclude ash, crude f1bre of cell wall or1g1n, phosphorous,

sulphur, potassium, z1nc, calc1um and phytate (Vose et a_l., 1976; Kon

et al., 1977; Reichert, 1981; Elkow1cz and Sosulski, 1982).

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Isolates, proteinates and micellar proteins.

In the fabrication of processed foods frequent use IS made of

Isolates. These isolates are of commercial Interest because they have

a bland appearance and taste, and Improved nutritional and functional

properties compared to flours and protein concentrates. They can be

used as protein supplements In cereal based foods ( eg. Thompson, 1977;

Fleming and Sosulski, 1977), or as functional Ingredients In processed

foods. Compositional, nutritional, functional and quality aspects of

soy Isolates have been assessed by Mattil (1974).

Soy Isolates generally have a protein content of greater than

90%. VIcia faba isolates and proteinates were produced with protein

contents of 87 and 83% (N x 5.7) respectively. This is slightly lower

than that of commercial soy Isolates, but compares with values

obtained for pea Isolates (Sumner et al., 1981). The Isolates were

cream coloured, but formed darker beige products when they were

neutralized. Fan and Sosulski (1974) and Fleming et al. (1975)

produced tan coloured Isolates from VI cia faba minor seeds. This was

presumably due to the presence ot pigments In the flours, and may be a

problem In the utilization of these products In some fabricated foods.

Sumner et al. (1981) suggested that coloured products were formed by

oxidation of polyphenols during freeze drying. Murray et a~. (1985)

reported a 0.84% phenolic acid content In dehulled VIcia faba flour,

and phenolic acids In flours and hulls and their Involvement 1n

producing coloured compounds was stud1ed by Sosulskl and Dabrowskl

(1984}. Fleming et al. (1975) suggested that phenol1c ac1ds are

oxidlzed to quinones, and complex Wlth proteins under alkal1ne

conditlons as descr1bed by Sab1r et al. (1974). This would explain the

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development of colour after neutralization to form the proteinate.

Micellar proteins with 98% protein (N x 5.7) were produced

from both Maris Bead and IVS-G flours. This compares with a value of

96% protein (N x 5.85) obtained by Murray et al. (1981). This is muCh

higher than the protein contents of isolates and proteinates, and

demonstrates the effectiveness of the method in excluding other

compounds, eg. llpids and phytate. The two methods used for preparing

micellar proteins yielded products with significantly different

characteristics. The micellar protein formed without ultrafiltration

precipitated very quickly when water was added. A thick gelatinous

mass was formed at the bottom of the beaker, as previously observed by

Murray et al. (1981). The freeze dried product was an off-white colour

and more dense than the isolate and proteinate preparations. However,

the micellar proteins formed after reduction of the supernatant by

ultrafiltration did not precipitate so quickly or form a thick viscous

layer in the bottom of the vessel. Precipitation was allowed to

proceed over-night in a cold room, but in some cases a centrifugation

step was necessary to collect the precipitated protein. The

freeze-dried product resembled the isolate preparation in appearance

and physical characteristics. It was considered to be more equivalent

to a isolate.

Proteinates, isolates and micellar proteins were analyzed by

SDS-PAGE and shown to be Chiefly composed of the major storage

proteins of Vicia faba., ie. legumin and vicilln (Figure 7). These

proteins account for 80% of the total seed protein In V.faba, and are

discussed In greater detail in the following section. Protein bands

observed by SDS-PAGE of the flours, but absent from proteinates,

Isolates and micellar proteins probably correspond to proteins from

the more soluble albumin fraction.

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To test the homogeneity of the preparations they were

subJected to gel filtration on Superose 6 (Figure 8). The micellar

protein preparation was d1fficult to get into solution, so was not

used. Insoluble material was removed by centr1fuging all of the

samples prior to testing. Therefore, only soluble aggregates were

observed. The largest anount of high molecular we1ght material (Mr.

approx. 3 million) was observed for the isolate. This probably

reflects a greater extent of protein aggregat1on, possibly induced by

ac1d prec1pitat1on. In these experiments severe but localized ac1d

denaturation was avoided by adding d1lute ac1d dropwise wh1lst

st1rring the sample. Arntfield and Murray {1981) demonstrated, using

DSC analyses, that some denaturation does occur during isoelectric

prec1pitation of Vicia faba proteins. Lillford and Wr1ght (1981)

observed that all of the soy prote1n precipitated at pH 4.5 could be

recovered by adJusting the pH to 7.6, providing that the sample was

freshly prepared. However, some of this protein may have been

denatured but st1ll reta1ned its solubility. Alternatively, V1cia faba

proteins may be more sensitive to isoelectr1c precip1tat1on. The

isolate also contained a large proportion of low molecular weight

species. These could have been e1ther dissoc1at1on products of the 7S

or llS components, low molecular weight proteins, eg. whey prote1ns,

or proteolytic breakdown products formed during extraction. Whey

proteins should rerna1n in solut1on during isoelectr1c precip1tat1on,

so their involvement is unllkely. The former explanation is the most

likely as SDS-PAGE revealed that most of the protein corresponded to

subunits of the major storage proteins. However, some proteolyt1c

breakdown products may also have been present, as some lo.v molecular

we1ght bands were observed by SDS-PAGE. Proteolytic breakdown products

from vic1l1n subunits have been 1dent1fied by Scholz et al. (1983).

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The isolates produced by ultrafiltration had small amounts of

low nolecular weight material. The pJre size in the membranes used

prov1ded a cut pJint of Mr. approx. 50 000. r.a.v nolecular weight

proteins would be renoved in the f1ltrate and only proteins in a

relat1vely native state reta1ned.

Although isolates, proteinates and micellar proteins have many

super1or quallties compared to prote1n concentrates, flours and grits

there are also some disadvantages associated with the1r product1on.

L1p1ds tend to concentrate with the protein fraction during

1solate and proteinate preparation, and may amount to 7.7 and 12% of

1solates prepared from defatted or full-fat flours respectively

(Wright and Bumstead, 1984). At these levels storage problems and

effects on funct1onality become more pronounced. Storage problems

emanate from the action of lipoxygenase on fatty acids to form

hydroperox1des, which may react further to form a w1de range of

volatile compounds, giv1ng rise to undesirable flavours and odours

(Gardner, 1975; Rackis et al., 1979). LipJxygenase has a strong

aff1n1ty for l1nole1c ac1d which accounts for 55% of the compJnent

fatty acids in Vic1a faba (Hinchcliffe et al., 1977). Faba bean

llpoxygenases have been isolated by Eskm and Henderson ( 1974) .

However, as most faba bean fatty acids ex1st in ester1f1ed form as

tr1acylglycerides and phospholipids the actions of l1pases and

phospholipases are also impJrtant. These enzymes have been isolated

and character1zed by Dundas et al. (1978) and Atwal et al. (1979).

Henderson et al. (1981) propJsed an overall mechanism for l1p1d

degradatlon 1n faba beans. Lip1ds and their degradation products can

b1nd to prote1ns and 1nterfere with functional propert1es. In some

cases 1t may be necessary to renove them us1ng spec1al solvent systems

(Wolt, 1975). These l1p1d protein complexes have been stud1ed by St.

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Angelo and Ory (1975) and St. Angelo and Graves (1986).

Drying of isolates, proteinates and micellar proteins can be

expensive. Also, the methcxi of drying has been shanrn to affect the

composition and appearance of pea isolates (Sumner et al., 1981).

Drum-drying resulted in isolates with a toasted flavour and darker

colouring. Freeze-drying prcxiuced Isolates with a cerealy flavour, and

was also implicated in the formation of coloured products.

Spray-drying produced isolates with the most bland flavour and

appearance. H011ever, sodium proteinates generally had superior flavour

characteristics compared to Isolates, but were darker in colour.

Finally, the production of whey type liquids during isolate,

proteinate and micellar protein production IS a potential water

pollution threat. This is also a perennial problem for the cheese

industry, as 20% of milk proteins are contained in the whey fraction

(Burgess and Kelly, 1979). However, whey proteins can be formed into

useful by-products using ultrafiltration to concentrate the useful

constituents (Lawhon et al., 1974). The resultant whey fraction can

either be used directly in animal feeds, or separated to yield a

soluble protein fraction, a soluble carbohydrate fraction and water

for recycling (Vose, 1980). Whey proteins have been shown to have

useful functional and nutritional properties (Burgess and Kelly, 1979;

To et al., 1985).

Ultrafiltration With small pore size membranes has been used

directly in the production of Isolates from cotton seed, field pea and

horse bean {Lawhon et al., 1977; 1978; Vose, 1980). These isolates

will also contain whey proteins, sugars and ash, so would be expected

to have different functional properties. The method also totally

avoids the need for effluent disposal.

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The effects of these processing methods on solubility and

denaturat1on are discussed in subsequent sections.

Characterization of Purified Proteins.

The subunit structure of Maris Bead legumin has previously

been studied by Maplestone et al. (1985). On non-reducing gels they

observed a d1stinct band corresponding to a Mr. of 56 000, and fa1nter

bands correspond1ng to Mr. values of 65 - 70 000 and 40 000. Similar

results were obta1ned 1n this study but the 40 000 Mr. band was more

d1st1nct and the bands correspond1ng to Mr. values of 65 - 70 000 were

e1ther very faint or 1ndiscernible (F1gure 10). Under reduc1ng

conditions maJor bands were observed corresponding to Mr. values of

36 000, 23 000 and 21 000. This is 1n general agreement with previous

stud1es (Wr1ght and Boulter, 1974; Maplestone et al., 1985).

Typ1cally purified vicilin does not migrate as a sharply

deflned band during electrophoresis under non-denaturing conditions

(Ilbuchi and Imahor1, 1978; Gatehouse et al., 1981). Vic1l1n from

V-faba in these experiments y1elded a s1ngle broad peak dur1ng gel

tiltrat1on and analyt1cal scann1ng ultracentrlfugation. Considerable

heterogeneity of vicil1n proteins has been demonstrated. Four maJor

subun1ts w1th Mr. values of 66 000, 60 000, 55 000 and 38 000 were

prcduced by SDS-PAGE. This 1s in agreement with the findings of Bailey

and Boulter (1972). The subunit pattern was not altered by

electrophores1s 1n the presence of 2-mercaptoethanol.

Legumin y1elded more than one peak by gel filtration and

dur1ng analytical scanning ultracentnfugation (Figures 11 and 12

respectlvely). Peaks 3 and 6 obta1ned by gel filtrat1on were ass1gned

a Mr. value of 600 000. Th1s was cons1dered to be a d1mer1zed form of

the llS prote1n. When the protein was subJected to SDS-PAGE 1t formed

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an 1dent1cal band pattern to that of the US protem. A small peak

Wlth an Sobs value of 14-16S was observed dur1ng analyt1cal

ultracentr1fugat1on. Thls was also attrlbuted to d1merized llS

prote1ns. Same much larger aggregates were also observed dur1ng gel

f1ltrat1on of legum1n preparat1ons, particularly in those samples

which were d1alyzed against distllled water. This could be expla1ned

by the format1on of d1sulph1de l1nkages after prec1p1tat1on dur1ng

d1alys1s, or dur1ng lyoph1llzat1on (Hoshl and Yamauchl, 1983). The

add1t1on of ammon1um hydrogen carbonate rendered the prote1n more

soluble. Sed1mentat1on coeff1c1ents were s1m1lar to prev1ously

reported values (Derbysh1re et al., 1976; Mori and Utsumi, 1979).

Solub1l1ty character1st1cs.

D1spers1bil1ty prof1les of Marls Bead and IVS-G prote1n

preparat1ons were simllar 1n character to those reported prev1ously

for peanut isolates (Rhee et al., 1973), soy 1solates (Shen, 1976a;

Hermansson, 1979), and mung bean, held pea, fababean, ch1ck pea,

lup1n, lent1l, pea bean and llma bean flours (Fan and Sosulskl, 1974).

M1n1mum n1trogen solubllity occurred at pH values between 4 and 6.

However, mung bean, held pea and soy bean had very narrow apparent

1soelectr1c po1nts, faba bean, chlCk pea and lupin had 1ntermed1ate

w1dth ones, and lentil, pea bean and llma bean had a broad m1n1mum

solub1l1ty range. The results presented 1n th1s thesis are not

d1rectly comparable w1th those 1n the l1terature as dlfferent prote1n

concentrat1ons and methods were used. It was necessary to use 10%

proteln concentratlon as gel format1on would not have occurred at

lower levels. At h1gher prote1n concentrat1ons m1n1mum proteln

solub1l1ty 1s lower than at lower prote1n concentrat1ons, and the

apparent 1soelectnc po1nt 1s broader (F1gures 14 and 15). Shen

(1976b) observed no effects on prote1n solub1l1ty us1ng concentrat1ons

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up to 10%. However, d1 fferent expenmental procedures were employed.

Sml th et al. ( 1966) and Betschart ( 197 4) d1d observe decreased

extractab1l1ty w1th 1ncreas1ng prote1n concentrat1ons up to 10% for

soy protein and leat protein respect1vely. Blend1ng speed,

ca~tr1fugat1on t1me and 1ntens1ty, equ1l1brat1on time, temperature and

ettect1veness of m1x1ng all affect the values obta1ned for solub1l1ty

(Shen, 1976b).

Max1mum n1trogen solub1l1ty was observed between pH values ot

2- 3.5 and >7 (F1gures 19-22). Net charge on the protein molecules 1s

h1ghest at these pH values, and so intermolecular repuls1ve forces

render the prote1n more soluble. Protein-proteln interact1ons are

favoured at 1ntermed1ate pH values, result1ng 1n some prote1n

preclpitation.

The proteinates were more soluble than the micellar prote1ns

over the entire pH range, although the latter were expected to be 1n a

more native state (Figures 19 and 21). Tne IVS-G m1cellar prote1n was

prepared by ultraflltration, and as discussed previously d1d not

exlnbit typical m1cellar protein characterist1cs. Extens1ve

prote1n-prote1n 1nteractions occur dur1ng m1celle formation and these

may be stabil1zed by subsequent d1sulphide bond formatlon, thus

render1ng the prote1n insolubl~ (Murray et al., 1981). Prote1n-prote1n

1nteractions were less extens1ve 1n the IVS-G preparation as rap1d

prote1n prec1p1tatian did not occur. Isolates would be expected to

have 1ntermed1ate solub1l1ty character1st1cs compared to proteinates

and m1cellar prote1ns. Thls 1s substantiated by prote1n contents of

the 20% solut1ons at two pH values (Table 13). Lillford and Wr1ght

(1981) demonstrated that d1sulph1de l1nkages are formed dur1ng storage

of soy isolates render1ng them less soluble. Thls could be reversed by

the add1t1on of reduc1ng agents. Decreased solubllity after

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1soelectr1c prec1p1tat1on of soy prote1ns has also been observed by

Nash and Wolf (1967}, Nash et al. (1971} and Anderson (1974}. Improved

solub1l1ty characteristics of prote1nates, as compared to 1solates,

have also been observed for leaf prote1ns (Lu and K1nsella, 1972:

Betschart, 1974}. Th1s can be attnbuted to a change 1n the surface

d1str1but1on of charge on the protein molecules caused by adJUSting

the pH, and the h1gher salt content of the proteinate. Both of these

factors 1ncrease solub1l1ty at the expense of prote1n-prote1n

1nteract1ons.

The use of solub1l1ty profiles as a measure of prote1n

denaturation 1s clearly not val1d 1n compar1ng these samples.

Furthermore, Hermansson (1979} reported that a completely denatured

soy 1solate could have a solubility prof1le s1m1lar to that of a

nat1ve soy 1solate. D1fferent1al scann1ng calorimetry (DSC} analys1s

1s a more rel1able 1nd1cator of denaturation, and has been used to

mon1tor the effects of process1ng on soy 1solates (Hermartsson, 1979),

f1eld bean 1solates and m1cellar prote1ns (Murray et al., 1981) and

t1eld pea, faba bean, soy and canola 1solates (Murray et al., 1985).

DSC analyses are d1scussed 1n the next sect1on.

Turb1d1ty values closely m1rrored n1trogen solub1l1ty levels.

However, h1gh turb1d1ty values were observed at relatively low prote1n

concentrations tor the Marls Bead m1cellar prote1n. Populations of

v1c1l1n micelles can undergo dynam1c interactions. The most extens1ve

network formations occur at pH 6- 7, where extens1ve prote1n sheets

are formed. As the pH 1ncreases these sheets may break up to form

small m1celles 1n aggregates or s1ngle m1celles wh1ch can ex1st 1n

solut1on (Ismond et al., l986a). S1m1lar populat1ons are the l1kely

cause of the h1gh turb1d1ty values observed (F1gure 21). However,

changes 1n turb1d1ty may be attributed to changes 1n the number, s1ze

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or opt1cal propert1es of part1cles.

Full-fat Marls Bead prote1nate was more soluble than the

defatted sample (F1gures 19 and 20). However, a large proport1on of

the protein was 1n solut1on 1n a collo1dal state. The apparent

1soelectr1c po1nt was also narrower than for the defatted sample. The

1nterference of lip1d-prote1n 1nteractions w1th prote1n-prote1n

interact1ons requires further 1nvestigat1on. St. Angelo and Graves

(1986) observed increased solubility of full-fat peanut prote1ns

compared to defatted samples. However 1t 1s poss1ble that the

defatt1ng procedure was respons1ble for the loss of solub1l1ty.

The d1fferences in sed1ment volume observed between

prote1nates and m1cellar prote1ns probably reflects the different

structural character1stics of the samples. M1cellar proteins may

undergo extens1ve coalescence to form amorphous three-d1rnens1onal

structures (Isrnond et al., 1986a). These would be expected to pack

very closely, result1ng 1n low sed1rnent volumes (F1gures 13, 14 and

17).

The effects of salt on the d1spers1b1lity character1st1cs of a

defatted Marls Bead prote1nate were 1nvest1gated at pH 7.7. In the

absence of salt v1rtually all of the prote1n was extracted. Increas1ng

the salt content to 2% caused a decrease 1n prote1n solub1l1ty (F1gure

24). The effects of salt are pH dependent. Herrnansson (1979) reported

a sharp decrease 1n the prote1n solub1l1ty of a soy prote1nate (pH 7)

when the salt concentrat1on was 1ncreased from 0 - O.lM. Ra1s1ng the

salt content to 0.4M increased prote1n solubllity. However, at pH 5

1ncreas1ng the salt concentrat1on 1ncreased solubil1ty from < 10% w1th

no salt to approx1mately 60% at O.SM salt. Furthermore, 1solates

exh1b1ted dlfferent behav1oural character1st1cs. Small concentrat1ons

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of calclum chlor1de also profoundly affect solUb1l1ty on the alkal1ne

s1de of the 1soelectr1c point (Hermansson, 1979). Th1s 1s of

part1cular sign1f1cance in the fabr1cat1on of milk type products.

The effects of temperature.

The effects of temperature on food prote1ns have recently been

rev1ewed by K1lara and Sharkas1 (1986). The use of heat m the

preparat1on of protein-r1ch products has been shown to have an adverse

eftect on the sUbsequent solUb1l1ty of prote1ns from m1lk whey (Morr

et al., 1973), soy beans (Wolf, 1970; Johnson, 1970), alfalfa leaves

(Betschart, 1974), blood {Tybor et al., 1975), cottonseed (Lawhon and

Cater, 1971) and great northern beans (Pllosof et al., 1981). However

the use of heat 1s frequently necessary to destroy ant1-nutr1t1ve

factors and 1mprove flavour character1st1cs.

Prote1n denaturat1on, caused e1ther by heat1ng or other

process1ng methods, can be measured us1ng DSC analysis. A large~

value 1nd1cates a relat1vely undenatured prote1n. Also the

determ1nat1on of denaturat1on temperatures for maJor bean components

ass1sts 1n pred1ct1ng the behav1our of products 1n ccx:>ked foods by

1nd1cat1ng the temperatures at whlch gell1ng or other maJor phys1cal

changes may occur.

The tust maJor peak observed for the bean flour had a Tmax

value ot 337. 7K, and was attnbuted to starch gelat1mzat1on {Table

20). The observed values of Tm and Tmax were 1n close agreement Wlth

prev1ously reported values for V1c1a faba (Bil1ader1s et al., 1980),

but lower than those reported by Wr1ght and Boulter (1980). Thls may

be attnbutable to the d1fterent types of bean used; faba bean, horse

bean and broad bean respect1vely. Starch gelat1n1zat1on 1s 1mportant

1n a nwnber of food processes, eg. the bak1ng of bread and cakes,

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extrusion, th1cken1ng and gell1ng. The observed starch gelatin1zat1on

temperature 1s also s1milar to that reported for corn and potato

starches (Blliaderis et al., 1980), suggest1ng that it may have

potent1al appl1cat1ons 1n foods where corn and potato starches are

conventionally used.

The trans1t1ons due to denaturation of v1c1l1n and legum1n

trom Marls Bead flour had s1milar values of Tmax to those reported

previously by Wr1ght and Boulter (1980). However, pur1f1ed prote1ns

had lower values of Trnax 1nd1cat1ng that they are somehow stab1l1zed

aga1nst denaturation in the flours, poss1bly due to differences 1n the

water env1ronment. Th1s phenomenon was previously reported by Wr1ght

and Boulter (1980). A broad peak was observed tor vic1l1n, 1nd1cat1ng

heterogeneity 1n th1s prote1n.

The h1ghest~H values were abta1ned for the m1cellar prote1ns

suggest1ng that th1s processing method produces the least denaturat1on

(Hermansson, 1979; Arntf1eld and Murray, 1981; Murray ~al., 1985).

The ultraf1ltrat1on product was also relatively undenatured. Isolates

and prote1nates were denatured to vary1ng extents, poss1bly due to

ac1d prec1p1tat1on or prote1n aggregat1on.

Other character1st1cs wh1ch have been used to measure the

extent of denaturation 1nclude a) opt1cal properties, measured by

opt1cal rotatory d1spers1on (ORO) or c1rcular d1chro1sm (CD) (Kato et

al., 1981; Matsuda et al., 1981), b) vis1ble and u.v. spectra

(Herrnansson, 1979), and c) fluorescence and polar1zat1on propert1es

(Yamag1sh1, 1982).

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Gelllng.

Many stud1es have been made on the factors 1nvolved in the

gell1ng of soy prote1ns. Cons1der1ng the structural s1m1larit1es

between legume proteins it is l1kely that s1m1lar mechan1sms are

1nvolved 1n the gell1ng of ~ faba prote1ns.

Heat1ng a solut1on of soy prote1ns produces an 1rrevers1ble

v1scous state ( PRCGEL) • Coollng may result m gel formatlon, although

th1s step may be reversed 1f heat 1S subsequently applled

(cats1mpoolas and Meyer, 1970). The use of salts, reduc1ng agents,

denaturants and water m1sc1ble solvents has y1elded informatlon on the

rnechan1srns 1nvolved 1n the soy prote1n gelat1on process (C1rcle et

al., 1964: Cats1mpoolas and Meyer, 1970: Hash1zume et al., 1975;

Sh1mada and Matsushita, 1980: Baba]1mopoulas et al., 1983: Utsuffil and

K1nsella, 1985a). These mechan1sms have been shown to d1ffer for gels

formed from e1ther a m1xed globul1n fract1on or 7S or llS fract1ons

(Hash1zume and Watanabe, 1979: Sh1mada and Matsush1ta, 1980: Utsum1

and K1nsella, 1985a; b; Herrnansson, 1985). These are swrnnanzed bela,..r.

The llS prote1n undergoes a thermal trans1t1on at 90°C

(Hash1zume and Watanabe, 1979: German et al., 1982). In d1lute

solut1ons the llS prote1n d1ssoc1ates 1nto subun1ts, and th1s 1s

followed by aggregat1on and prec1p1tat1on of the bas1c subun1ts, due

pr1mar1ly to hydrophob1c 1nteract1ons. Th1s prec1p1tat1on 1s enhanced

1n the presence of low concentrat1ons of 2-mercaptoet~l

(catslmpoolas et al., 1967: Wolf and Tamura, 1969: Catsimpoolas et

al., 1970: Catslmpoolas and Meyer, 1970; Mor1 et ~!·, 1981a: German et

al., 1982: Utsum1 ~a!., 1984). At prote1n concentrat1ons of

approX1mately 14% gelllng may occur. Two mechan1sms for gel format1on

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have been proposed. Nakamura et al. (l984b; I985a) and Mon et al.

(l98la) suggested that heating causes only minor changes to the

quaternary structure of the llS ol1gomers. The llS proteins polymerize

to form strands which interact to form macroaggregates, wh1ch form the

gel network. Hermansson (1985) suggested that d1ssociat1an occurred by

the same mechan1sm as in dilute solutlons, but there was no separat1on

1nto ac1d1c and bas1c subun1 ts. Subun1 t paus reassociated to form

strands wh1ch were equ1valent to the polymer1zed aggregates observed

by Nakamura et al. (l984b) and Mor1 et al. (l98la). The strands were

bu1lt up of hollow cyl1nders Wlth an external diameter of 12-15 nm

(Hermansson, 1985). The format1on of strands as a result of

aggregat1on, followed by 1nteract1on of the strands to form a gel

matr1x has been observed for other globular proteins (Tombs, 1974).

The contr1but1on of 1nd1v1dual ac1d1c subun1ts to gel

format1on 1s not un1form. In part1cular ac1dic subun1t III (ASIII) has

been shown to promote gel hardness 1n reconst1tuted pseudoglyc1n1ns

from a) 1solated ac1dic subun1ts +total bas1c subun1ts (Mor1 et al.,

1982), and b) from 1ntermediary subun1ts (Nakamura ~~l·, l985b).

Utsum1 and K1nsella (l985b) demonstrated that ASIII was d1ff1cult to

solub1l1ze from gels. S1m1larly ASII has been shown to contr1bute to

gel hardness 1n reconst1tuted pseudoglycimns from broad bean (Utsuml

et al., 1983). Conversely, ASIV contr1buted marg1nally to gel

tormat1on. JlSIV 1s the rost ac1dic of the ac1d1c subun1ts, and 1s not

llnked to 1ts correspond1ng baslC subun1t by a d1sulph1de bond (Mon

et al., l98la; 1982). However, 1ts presence has been shown to reduce

by half the t1me requued for gelllng to occur. Thls has been

attr1buted to the more heat-lab1le nature of the non-covalent l1nkage

between the ac1d1c and bas1c subun1ts, result1ng 1n conformat1onal

changes 1n glyc1n1n wh1ch st1mulate. the format1on of soluble

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aggregates, and subsequent p:::>lymenzat1on (Mon ~~~-·, 198la). The

release of ASIV tram glycinln dur1ng heat1ng has been rep:::>rted (Mor1

et al., 1982; Nakamura et al., 1984a; 1985a). Furthermore 1t 1s the

most read1ly solubil1zed ac1d1c subun1t from preformed gels {Utsumi

and Kinsella, 1985b).

The gelling mechan1sm of the 75 prote1n has been less well

stud1ed. The 75 prote1n undergoes a thermal transition at a lower

temperature than the ll5 protem (Table 20). Gel formation will occur

at a lower temperature {80°C) and prote1n concentrat1on (approx. 11%)

than for 115 prote1ns {5hlmada and Matsush1ta, 1980). No d1ssoc1at1on

products have been 1dent1f1ed dur1ng gel format1on of 75 prote1ns, and

1t 1s thought that aggregat1on occurs without pr1or d1ssoc1at1on

(Hashlzume et al., 1975). Heat1ng causes a greater v1scosity 1ncrease

than for 115 prote1ns, however, viscos1ty does not 1ncrease as much

dur1ng coollng (BabaJimopoulas et al., 1983). Hydrcx:Jen bonds are

bel1eved to be· the rost 1mp:::>rtant factor 1n the format1on of hard and

elast1c gels from 75 prote1ns (BabaJlmop:::>ulas et al., 1983; Utsum1 and

K1nsella, 1985a). All three of the 75 subunlts appear to contnbute

equally to gel tormation (Utsum1 and K1nsella, 1985a; b). The network

structure for 75 proteins has been reported to be denser and rore

cross-llnked than that of 115 prote1ns (Hermansson, 1985). Many

authors have reported d1fferences 1n the gell1ng propert1es of 75 and

115 prote1ns (8a1o and Watanabe, 1973; 8a1o et ~1., 1974; Hash1zume et

al., 1975; 8h1mada and Matsushlta, 1980; BabaJlmop:::>ulas et al., 1983;

Utsum1 and K1nsella, 1985a; b). However, these must be treated w1th

caut1on. Many of the 75 preparat1ons used have been only 70% pure and

have conta1ned large quant1t1es of contam1nat1ng 115 prote1n.

Furthermore, the presence of calclum ions 1n preparat1ons has been

shown to have a profound effect on gell1ng propert1es (5kurray et al.,

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1980).

Gels formed from a 1:1 mixture of llS and 7S prote1ns have

superior gelling properties to either ind1vidually {BabaJ1mopoulas et

al., 1983). When d1lute solut1ons of 7S and llS proteins are heated

there 1s no aggregat1on or prec1p1tat1on of the llS bas1c subun1ts

(Hash1zurne and Watanabe, 1979; German et al., 1982). Ha-~ever, 1f salt

1s present aggregat1on and prec1p1tat1on may occur (Hash1zurne and

Watanabe, 1979). In the absence of salt soluble complexes are formed

between the bas1c subun1ts of the llS prote1n and conglyc1n1n via

electrostat1c 1nteract1ons (Darnodaran and K1nsella, 1982). D1sulph1de

bonds may also form between bas1c subunlts {Utst.mu et al., 1984;

Yarnag1sh1 et al., 1984). The~ subun1t of conglyc1n1n was involved 1n

complex forrnat1on to a greater extent than the ex or a 1

subun1 ts

(German et al., 1982; Utsurn1 et· al., 1984; Utsurn1 and K1nsella,

1985b). However, 1n more concentrated solut1ons all of the conglyc1n1n

subunlts appear to be equally involved in gel structure format1on

{Utsurn1 and K1nsella, 1985a). The maJor factors involved in gel

format1on were hydrogen bonds and hydrophob1c 1nteract1ons. D1sulph1de

l1nkages were not necessary for gel format1on, but may contr1bute to

gel elast1c1ty (Furakawa and Ohta, 1982; BabaJimopoulas et al., 1983;

Utsurn1 and K1nsella, 1985a). ASIII was aga1n 1nvolved 1n gel format1on

and hardness (Utsurn1 and Kinsella, 1985a).

Gell1ng of V. faba prote1ns was favoured at pH values of 2.5 -

3.5 and 6 - 8, and was least favoured at pH values of <2.5, 4 - 5.5

and >10 (F1gures 13-18). Close to the 1soelectr1c po1nt (pH 4 5.5)

prote1n solub1l1ty 1s very low and so gel format1on 1s l1m1ted by

prote1n concentrat1on. A s1m1lar decrease 1n gelling ab1l1ty at

extremes of pH has been observed by Cats1mpoolas and Meyer {1970).

Electrostatic 1nteract1ons between the bas1c subun1ts of the llS

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prote1n and v1c1l1n subun1ts are 1nh1b1ted at extremes of pH, and the

prote1ns tend to rema1n in solut1on.

M1cellar proteins formed strong gels at pH 3.5 desp1te hav1ng

a low protein solubil1ty (F1gure 17). Gels were also formed at pH

values >8. All micellar protein gels had a highly aggregated

structure. Murray et al. (1981) reported that micellar prote1ns tend

to form f1bres 1n aqueous env1ronments, and that these f1bres can be

heat coagulated. The forrnat1on of f1bres 1n solut1on could prov1de the

bas1s tor rnatr1x format1on.

The full-fat Marls Bead prote1nate formed gels at a w1der

range of pH values than the defatted sample. Sh1mada and Matsush1ta

(1981) observed that soy prote1n gels formed with added o1ls were

always f1rmer than those produced w1thout oil. The l1p1d content of

the samples was not determined, but l1p1d contents of 12% have been

reported for pea 1solates (Wright and Bumstead, 1984). Cats1mpoolas

and Meyer (1971) reported that add1ng up to 40% mono-, d1- or

tr1glycer1des increased gel strength. Generally v1scos1ty was

increased by a) decreas1ng the chain length of the fatty ac1ds,

b) decreas1ng the ester1f1cat1on of hydroxyl groups on the glycerol

component, or c) 1ncreas1ng the degree of saturat1on. Phosphol1p1ds

and cholesterol were also shown to enhance gelat1on. G values and

rupture strength were also h1gh for gels produced from full-fat

samples (Table 12).

The effects of salt on gell1ng.

Gel strength 1ncreased w1th 1ncreas1ng salt content up to

1.25% (approx. 0.2M) for Marls Bead prote1nate (F1gure 23). Herrnansson

(1978) reported that thermal aggregates were formed dur1ng heat1ng of

soy prote1ns 1n O.lM NaCl, and thermal aggregat1on was max1m1sed at

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0.2M NaCl. Ra1s1ng the salt content further suppressed aggregatlon.

Other stud1es have reported a decrease 1n v1scos1ty by increas1ng salt

content from 0 - 2M at pH 7 - 8. The observed decrease was attnbuted

to the stab1l1zat1on of the quaternary protein structure aga1nst

dlssoc1at1on, thus afford1ng protectlon from thermal unfolding

(Catslmpoolas and Meyer, 1970; Hermansson, 1978; Baba]lmopoulas et

al. , 1983) • However, no measurements were recorded between 0 and 0. 2M

NaCl 1n these stud1es.

All of the gels formed were translucent, with the except1on of

those contain1ng 1.5 and 1.75% NaCl. However, the gels were dark brown

1n colour. The p1grnents respons1ble for th1s colourat1on were not

1dent1f1ed. However, 1t may prove necessary to remove them before the

prote1ns can be used 1n focd products.

SEM of gels.

Protein contents after centr1fug1ng of the 20% prote1n

solut1ons were all low, espec1ally for the micellar prote1n (Table

13). Thls was partly attr1buted to d1ff1cult1es 1n wett1ng the

samples, and partly to poor solubillty. All of the gels appeared to be

composed of h1ghly aggregated structures, particularly those of the

prote1nates and 1solates 1n wh1ch spher1cal aggregates of

approx1mately 12.5 ~m d1arneter were observed. These are much larger

than those reported by Herrnanssan (1985) 1n soy protein gels. She

reported strands w1th a d1arneter of 12-15 nm. However, the relevance

of the observed structures 1s doubtful, as using glutaraldehyde as a

f1xat1ve has been 1mpl1cated 1n the 1nduct1on of aggregated structures

1n prote1n gels (Herrnanssan and Buchhe1m, 1981).

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Rheolog1cal propert1es.

~g1d1ty of the gels was h1ghest at pH 4 and 4.6 (Table 12}.

These gels were opaque and pasty. Closer exarninat1an revealed that

they had l1ttle cohesion. The h1gh r1gid1ty values obta1ned were

probably due to structural compact1on dur1ng compression, and further

ernphas1zed by the 1ncreased cross sectional area produced by

compress1on (Calzada and Peleg, 1978}. Compression was accompan1ed by

syneres1s 1nd1cat1ng that the protein rnatr1x was coarse and had a low

water hold1ng capac1ty. The nature of the gel network 1s partly

determ1ned by the relat1ve rates of the denaturat1on and aggregat1on

steps. If aggregat1on 1s relat1vely slow a gel w1th a f1ner network of

prote1n cha1ns 1s formed. The resultant gel w1ll tend to be

translucent and elast1c. However: 1f aggregat1on 1s relat1vely fast a

coarse and 1nelast1c gel 1s formed. At pH values close to the

1soelectr1c po1nt the latter 1s favoured (Hegg et al., 1979; Hegg,

1982}. At pH 7 the protein 1s more soluble, and so the aggregat1on

process 1s slower. Translucent and relat1vely elast1c gels were formed

at th1s pH. Generally soft gels were produced at all pH values, even

at 20% sample concentration. Soy proteins have been shown to have

super1or gell1ng properties to bean proteins (Flem1ng et al., 1975;

Utsum1 et al., 1983). However, the 1ncrease 1n viscos1ty of heated

broad bean globul1n solut1ons was equ1valent to that of soy prote1ns

(Flem1ng et al., 1975). v. faba prote1ns may have a greater potent1al

1n m1xtures of gell1ng agents designed to g1ve a range of funct1onal

propert1es. The compatab1l1ty of broad bean llS prote1n w1th gelat1n

1n gell1ng systems has been 1nvest1gated by Andersson et al. (1985).

All polymer d1spers1ons are v1scoelast1c by nature, 1e. they

exh1b1t sol1d-l1ke elast1c and flu1d-l1ke v1scous behav1our

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simultaneously (Tung, 1978: Mitchell, 1980). Th1s 1s Important where

materials are exposed to constantly chang1ng forces as in chewing,

mashing, cutt1ng, m1xing, pouring, spreading or pump1ng. In a

stress-relaxation experiment the sample 1s subJected to a constant

stra1n and the res1dual stress 1s measured aga1nst t1me. The stress

1nduced 1n the sample can relax by several methods: a) v1scous flow of

polymer un1ts, b) breakage or format1on of chemical bonds, and

c) ster1c movement of polymer s1de cha1ns. Relaxation t1mes are

s1gn1ficant to the consumer 1f they operate over t1me penods wh1ch

are applicable to the act of mastication, 1e. relaxation t1mes of less

than 1 second. These may alter the consumer's perception of firmness.

The pr1nc1pal component of stress-relaxation 1s believed to be v1scous

flow (Bohlin, 1980). Three flow processes were 1dent1f1ed 1n the

protein gels (Table 14). However, 1t was not poss1ble to 1dent1fy them

w1th spec1f1c processes. Th1s has been successfully done for wheat

gluten dough (Mita and Bohl1n, 1983). Gluten has two flow processes

w1 th ccr-ordinat1on numbers of 4 and 2. Electron microscopy has

revealed that gluten is composed of non-aligned fibrillar structures

(z = 4) arranged to form a lamellar superstructure (z = 2) (Bernardin,

1975). Co-ordination numbers were var1able for prote1n gels, and the

appl1cab1l1ty of the theory to such gels 1s questionable as 1t 1s

unlikely that a s1mple ccr-operat1ve flow un1t is Involved (Table 15).

SEM of soy protein gels suggests that the strands are extensively

cross-l1nked (Herrnansson, 1985). The Intercepts of the F/F~ axes of

the rate - force plots gave pos1t1ve values. Th1s 1nd1cates that the

system was not 1n a state of equ1l1br1um pr1or to test1ng, and

ver1f1es the existence of cross-linkages and aggregates 1n the gels.

The above factors partially arrest flow processes, and cause Increases

1n relaxation t1mes and co-ord1nation numbers (Mlta and Bohlin, 1983).

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Foaming

Two factors contribute to the foaming propert1es of a

solut1on: a) foam expans1on, and b) foam stab1l1ty. These foam1ng

propert1es depend on the ab1l1ty of a surfactant to a) rap1dly ffilgrate

to a new 1nterface, b) to effect1vely lower 1nterfac1al tens1on at the

1nterface, and c) to stab1l1ze the 1nterface. The first requ1rement is

largely dependent on the d1ffus1on coeff1c1ent of the prote1n, and

generally smaller prote1ns w1ll reach the interface fastest

(MacR1tch1e, 1978). The 1nterface 1s a h1ghly denatur1ng env1ronment

for proteins. The reduct1on 1n interfac1al tens1on 1s ach1eved by an

1ncrease 1n surface pressure due to the protein orientating and

spread1ng 1tself at the interface. To fac1litate th1s a s1gn1f1cant

proport1on of exposed hydrophob1c surface and an ab1l1ty to rap1dly

unfold are des1rable (Graham and Ph1ll1ps, 1979a; b; Kato and Naka1,

1980; K1m and K1nsella, 1985). Once a monolayer has been formed

subsequent assoc1at1on of prote1ns with the 1nterface requ1res the

ab1l1ty to adsorb onto and insert into the pre-ex1st1ng f1lm w1thout

d1srupt1ng the f1lm's 1ntegr1ty. Adsorpt1on occurs cont1nuously where

e1ther stretch1ng of the f1lm due to bubble rearrangements or gas

d1ffus1on, or removal of prote1ns due to coagulat1on occur.

Coagulat1on commonly occurs at ag1tated air water 1nterfaces.

Prote1n molecules are converted to 1nsoluble part1cles wh1ch lose

the1r foam1ng propert1es causing the foam to collapse. Coagulat1on 1s

enhanced close to the isoelectric po1nt. Ovalbumin 1s part1cularly

suscept1ble to coagulat1on (Henson et al., 1970), and prec1p1tated

ovalbum1n has been observed 1n whipped egg wh1te (De V1lb1ss et al.,

1974). Adsorpt1on on to the 1nterface requ1res a tendency to b1nd to

hydrophob1c surfaces, and 1s enhanced close to the 1soelectnc pomt

where prote1n prote1n interact1ons d01n1nate. For the same reason

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foam strength 1s max1m1zed close to the 1soelectr1c po1nt, or at the

1soelectr1c po1nt for prote1ns wh1ch remain soluble (Buck1ngham, 1970;

MacR1tch1e, 1978; Hall1ng, 1981; Kinsella, 1981; Kim and K1nsella,

1985). No attempt was made to opt1mize cond1tions for each prote1n 1n

th1s study.

Samples l1ke a-casein and sod1um case1nate consist of small

and soluble molecules wh1ch can rap1dly migrate to the 1nterface. On

reaching the interface the readily ava1lable hydrophobic segments and

the molecular flex1b1l1ty of the protein fac1l1tates or1entat1on and

spread1ng at the 1nterface (Merc1er et al., 1971; Rlbadeau-dumas et

al., 1972; Merc1er et al., 1973). As Judged by 1n1tial conduct1v1ty

during sparg1ng a-case1n produced the greatest volume of foam (Table

16) . Tornberg ( 1978a; b) has prev1ousl y demonstrated the ab1ll ty of

a-case1n to form large volumes bf foam cons1st1ng of many small

bubbles. convent1onal measurements of foam volume do not account for

bubble s1ze. The advantage of the conduct1vity method is that 1t g1ves

an estlmate of the total volume of flu1d held 1n the foam. BSA and

hemoglob1n also formed large volumes of foam. BSA also has a hlgh

hydrophob1c1ty value and is relatlvely unstructured. The pH used for

the foaming exper1ments was close to the isoelectr1c point of

hemoglobin, myoglob1n and 'Y-globulln. HemOJlobin and myOJlobin both

produced br1ttle foams with large bubbles, poss1bly caused by

coagulat1on of prote1ns at the interface. The large foam volume

produced by wh1pp1ng the heiOCJg'lob1n sample does not accurately reflect

1ts foam1ng propert1es as bubble s1ze 1s not cons1dered. The measures

of foaming power obtained by the sparg1ng method probably more

accurately reflect the foam1ng power of hemoglob1n.

Prote1ns w1th a h1gh degree of tert1ary or quaternary

structure tend to res1st unfold1ng. A larger energy input 1s necessary

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to torm toarns fran these proteins, eg. lysozyme, ovalbumin and

~-globulin (Kato et al., 1983a: German et al., 1985). In this study

all proteins were foamed with an equal energy Input. It is assumed

that this was Insufficient for adequate film formation by lysozyme as

only a small volume of foam composed of large bubbles was formed

(Table 16). Soy proteins and v. faba proteins have compact quaternary

structures. The relatively poor foaming properties of soy proteins

have been attributed to the difficulties Involved In the adsorption

and unfolding of the protein at the air - solvent Interface (Tornberg,

1978a). In the native state soy proteins have a low value.of surface

hydrophobicIty ( Kato and Nakai, 1980) • Furthermore, unfoldmg Is

prevented by disulphide linkages. Treatment With a disulphide cleaving

agent facilitates unfolding and also results in the exposure of

hydrophobic residues, partlcul~ly on the basic subunits (German et

al., 1982: 1985). A dramatic improvement m foam expansion was

observed when soy proteins were treated with sulphite (German et al.,

1985). Soy hydrolysates are widely used as foaming agents in the food

Industry (Eldridge et al., 1963). Greater foam expansion has been

observed for hydrolysed soy proteins (Eldridge et al., 1963: Puski,

1975), egg white (Grunden et al., 1974) and whey proteins (Kuehler and

Stine, 1974).

Foams tend to be highly unstable because of surface tension.

For a film to be relatively stable the proteins must be a) able to

form a cohesive network capable of retarding film coalescence and

collapse of bubbles, b) capable of withstanding minor shocks due to

bubbles bursting, and c) able to repel the approach of adJacent fllms

(MacRitchie, 1978: Graham and Phillips, 1979a). A newly formed foam IS

composed of undistorted spherical bubbles. However, Initial rapid

drainage under the Influence of gravity causes these to distort and

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become polyhedral. Subsequent dra1nage may e1ther occur from plateau

borders at bubble 1ntersect1ons under the influence of gravity, or

from the lamellar regions between bubbles 1nto the plateau borders due

predom1nantly to Laplace cap1llary pressure. The latter force 1s

opposed by the negat1ve pressure 1n the plateau borders and double

layer repuls1ve forces between adJacent f1lms. Dra1nage of l1qu1d from

the lamellar reg1ons causes the 1nterfac1al f1lms to become th1n and

frag1le, and fac1l1tates gas d1ffus1on from small bubbles to larger

ones result1ng 1n the collapse of the bubbles (Halllng, 1981;

Klnsella, 1981). The fllm strength depends on rheolog1cal and adheslVe

propert1es, eg. surface topography, mechanlcal strength,

v1scoelast1city and water b1nd1ng capac1ty (Graham and Ph1ll1ps,

1979a). Generally prote1ns with a large molecular weight and a h1gh

degree of tert1ary and quaternary structure form more stable foams.

The bean and pea globullns produced the most stable foams, as measured

by the sparg1ng method. Th1s reflects the1r compact quaternary

structure. Isolates, prote1nates and ultraflltration products also

produced relat1vely stable foams (Table 16). Micellar prote1ns only

produced small quant1t1es of foam, probably due to the1r poor

solub1l1ty character1st1cs. Stable foams were also produced by sodlum

case1nate, BSA and soy whey prote1n. Sod1um case1nate read1ly forms a

v1scous solut1on wh1ch enhances foam stab1lity (Morr, 1981). However,

BSA and whey prote1ns do not usually form stable foams (German et al.,

1985). Under the cond1t1ons employed it would appear that 1nsuff1c1ent

adsorpt1on and denaturatlon

format10n Of VlSCOUS fllmS

ovalbum1n and ~-globul1n.

occurred at the 1ntertace for the

from the more structured prote1ns, eg.

No real d1tferences in foam1ng propert1es were observed

between 7S and llS prote1ns from peas and beans. The observed

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d1tferences were probably due to relat1vely minor d1fferences in

processing cond1t1ons. Also, there was no preferential retent1on of 78

compared to llS prote1ns, or vice versa, 1n foams produced from Marls

Bead 1solates (Figure 37). Poole et al. {1984) demonstrated that

lysozyme was strongly involved in matr1x format1on in egg albumen

foams. Th1s was attr1buted to electrostat1c interact1ons between

lysozyme and other more ac1d1c proteins.

Of the soy proteins tested the whey prote1ns had the best

foarru.ng propertles (F1gure 28). Whey prote1ns tend to be small,

soluble and capable of produc1ng large volumes of foam with a small

energy 1nput. However, they also tend to produce less stable foams

than globul1n prote1ns.

The effects of l1p1ds on foam1ng propert1es are clearly

demonstrated by comparing the results for the full-fat and defatted

soy flours (Table 16). Eldr1dge et al. (1963) demonstrated that polar

lip1ds were more detr1mental to foam format1on than neutral l1p1ds,

presumably due to the1r greater surface act1v1ty. Although l1p1d

contents are much lower 1n peas and fleld beans compared to soy beans,

isolates and prote1nates may conta1n apprec1able amounts of llp1d. The

effects of these are clearly demonstrated 1n both wh1pp1ng and

sparg1ng exper1ments.

Foam1ng propertles 1n defatted pea, bean and soy samples

1mproved w1th 1ncreas1ng prote1n content. The hlgher prote1n contents

of soy flours and 1solates compared to those of pea and bean probably

account for the super1or foam1ng characterist1cs (F1gures 30 and 32).

Values for foam expans1on deterffilned by the sparg1ng and

wh1pp1ng methods were not strongly correlated (Table 17) . As mentloned

prev1ously values for foam expans1on determ1ned by the wh1pp1ng method

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do not ind1cate the volume of l1qu1d held 1n the foam. A relatively

weak foam composed of large bubbles may have a greater volume than a

dense foam composed of many small bubbles. The conductiv1ty method is

probably a better 1nd1cator of foam qual1ty. Kato et al. (1983b)

reported that foam volume and initial conductivity were correlated.

However, h1s toam volume measurements were produced by sparging, and

not wh1pp1ng. In the exper1ments reported 1n th1s study only small

d1tferences 1n foam expans1on after sparg1ng were observed (Table 16).

However, d1fferent operat1ng procedures were used. Foam stab1l1ty

values produced by the two methods were more strongly correlated.

In conclus1on, the sparg1ng method was cons1dered to be a

better test of foam1ng propert1es for such camparat1ve exper1ments.

Increasing the v1scos1ty of the bulk solut1on should enhance

foam stabil1ty, although 1t may also be detr1mental to the rate of

foam format1on by decreasing the d1ffus1on rate of the prote1ns. It

has also been suggested that low concentrat1ons of sucrose enhance

foam1ng by creat1ng an unfavourable env1ronment for proteins, lead1ng

to prote1n deposition at the interface (Lee and Tlmasheff, 1981).

However, add1ng up to 12% sucrose to a solut1on of Marls Bead

prote1nate sl1ghtly reduced both foam expans1on and foam stabillty

(Table 18).

1nsuft1c1ent

Presumably the

to compensate

energy

tor the

1nput dur1ng foaming was

1ncreased v1scos1ty of the

solut1on. At concentrat1ons greater than 12% the heavy consistency of

the solut1on inhlbited foam format1on.

Partial denaturation of proteins has also been used to

Increase v1scos1ty as a means of 1mprov1ng foam stab1l1ty of egg

prote1ns (De V1lb1ss et al., 1974), whey prote1ns (Kuehler and Stine,

1974; Rlchert et al., 1974) and soy prote1ns (Eldrldge et al., 1963).

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Emulsifying properties.

The mechanics of emulsion formation are similar to those of

foams, Ie. a) diffusion of protein molecules to the Interface where

they are adsorbed In native form, b) surface denaturation of the

adsorbed protein, and c) aggregation of the denatured protein into a

coagulum devoid of surface . activity which is forced out of the

Interface by the spreading pressure of native protein undergoing

denaturation at the interface. If coagulation IS extensive the

coagulum may form a skin which will stabilize the emulsion (Acton and

Saffle, 1970).

Emulsifying profiles have been correlated with solubility

profiles for various proteins (Swift et al., 1961; Hegarty et al.,

1963; Crenwelge et al., 1974; Sosulski et al., l976b; Volkert and

Klein, 1979). The latter authors observed that emulsifying capacity

was not greatly affected when dispersible nitrogen was equalized over

the whole pH range. In this study emulsion activity was as follows

proteinates > Isolates > micellar proteins > prot.ein concentrates >

flours. Dispersible protein followed the same order. However, high

values for nitrogen solubility Index (NSI) are not necessarily

Indicative of good emulsifying properties (Smith et al., 1973;

McWatters and Holmes, l979a; b). Surface hydrophobicity together with

solubility characteristics are considered the best Indicator of

emulsifying properties by Voutsinas et al. (l983a).

Flint and Johnson (1981) reported that scy proteins could form

films at pH values below the Isoelectric point and up to a value of

7.5. This range Includes most food systems and all meat emulsions. In

studies on soy beans, 7S proteins have been attributed With superior

emulsifying properties compared tollS proteins (Aoki et al., 1980;

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Yamauchi et al., 1982). However, in this study llS prote1ns performed

sl1ghtly better than 7S prote1ns. Different methods of protein

preparat1on, different species and different methods of determining

emulsifying properties were used in all of the investigations.

The lowest values of EC and FA were obtained at the

1soelectric pH for soy 1solates and 7S proteins (Franzen and Kinsella,

1976: Kamat et al., 1978: Ramanatham et al., 1978: Volkert and Klein,

1979; Aoki et al., 1980). However, the llS protein had the lowest

values of EC and ES at pH 7. In this study emulsion activity was

determ1ned at one pH value only (pH 7 .5), and the US protein from

Maris Bead emulsified almost all of the ava1lable oil (Table 19).

Full-fat samples generally had Improved emuls1fying properties

compared to equivalent defatted samples (Table 19). Lipids generally

improve the emulsifying capaclties of proteins (Wang and Kinsella,

1976; Sosulski et al., 1976b). Hall1ng (1981) suggested that lip1ds

may act co-operatively with proteins during emulsiflcation. Many \

llp1ds contain small molecule surfactants, eg. mono-glycerides and

free fatty acids.

Products w1th h1gh protein contents generally had the best

emulsifying properties {Tables 3, 9, 10 and 19), suggesting that under

the conditions employed protein load was insufficient to test the

surface activity of the proteins. Halling (1981) observed a sharp

increase In emulsifying capacity with 1ncreasing protein content up to

a critical value, after which only small increases in emulsifying

capacity were observed. Differences between soluble prote1ns were

considered to be small. However, emulsifying propert1es could not be

explained by protein content alone. F1bre has been negat1vely

correlated with emulsifying properties by Yasumatsu et al. {1972).

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Coarse fractions generally had low values of emulsion activity,

presumably due to the presence of hull material.

The bean proteins had much higher FA values than casein. The

casein preparation used was prepared by rennet treatment and acid

precipitation. The resulting product IS highly insoluble and retains

the original calcium content of the native casein m1celle. It IS

non-functional as an emulsifier unless the calcium 1an content is

reduced. The emulsifying properties of a~1 -casein and its hydrolytic

derivatives have been studied by Shimizu et al. (1983).

The soy Isolate performed better than bean and pea 1solates

and proteinates. This possibly reflects Its slightly higher protein

content, although the methcd of prcduction may also have been

Important. Aoki et al. (1980) and Ochlai et al. (1982) observed

Increased values of EC over the pH range 2 - 10 for hydrolysed soy

proteins. ThiS was attnbuted to elther Improved solubility

characteristics, or exposure of more hydrophobic residues. Heat

denaturation and llpophillza.tion have also been reported to 1mprove

the emulsify1ng properties of soy proteins by Kamat et al. (1978) and

Aoki et al. (1981) respectively. However, muscle proteins are

considered the best emulsifying agents (Smith et al., 1973).

The difficulty of extrapolating from model systems to actual

focd systems with many Interacting components is significant. Puski

(1976) has suggested that three different methods for evaluating food

additives as emulsifying agents should be used, depending an the type

of product be1ng developed, Ie. a) comm1nuted type meat systems,

b) low fat m1lk type systems, or c) h1gh fat mayonna1se type systems.

For 1nclusion 1n cooked meats temperature dependance, water bind1ng

and gelat1on are also 1mportant. Vaisey et al. (1975) used faba bean

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and tield pea prote~n concentrates as ground beef extenders ~n

patt~es. It was necessary to textur~ze the protein to produce samples

s~m~lar to the beef controls. 30% soy protein substitution ~s poss~ble

1n ground beef and turkey loaves without caus~ng adverse effects on

fat content, water hold~ng capac~ty, texture and flavour (W1ll1ams and

Zab~k, 1975). However a potential problem associated with add~ng soy

proteins to meat systems 1s the development of ranc1d flavours due to

the ox~dat~on of l~p~ds. Th~s 1s part~cularly signif1cant 1n poultry

products wh~ch have a large unsaturated fat content. The use of

non-meat meat extenders has recently· been reviewed by M~ttal and

Osborne (1985).

Conclus~on

In th~s study var~ous process1ng methods were used to produce

prote~n or starch enr~ched products wh~ch were then assessed for

tunctional~ty ~n model tests. The processing methods used were

defatt~ng, a~r class~f~cat1on, and product1on of 1solates, prote~nates

and m~cellar prote~ns. These ranged in prote~n content from 33 - 98%.

A starch concentrate contain~ng 60% starch was also produced.

The relatively h~gh prote~n content of v. faba seeds make them

an ~deal mater1al for produc~ng large y1elds of high prote1n content

products. Equ~valent pea products tend to have lower prote1n contents,

or can only be produced 1n low y1elds. However, the super1or protein

content and funct~onal1ty of defatted soy flours compared to those of

v. faba w1ll make 1t d~ff1cult for the latter to compete 1n the same

markets. Prote1n concentrates produced by air class1f1cat1on were more

equ~valent 1n prote~n content to defatted soy flours. However, they

d1d not exh~blt equ~valent funct1onal1ty 1n foam~ng tests. Th~s was

attr1buted to a h1gh llp~d content.

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~r classification was used to produce fractions enriched in

protein, starch and hull material. The technique has many advantages

compared to conventional wet processing methods, including being able

to avoid the use of potential protein denaturants, thus leaving the

protein In Its native state, and obviating the need to dispose of

effluent. However, a maJor problem is the tendency of lipid to

fractionate with the protein fraction. Defatting using solvents to

extract the polar lipids may have a detrimental effect on protein

functionality. Raffinose and stachyose also fractionate w1th the

prote1n, and may affect the market potential of the product.

Impact m1ll1ng efficiency was lower for IVS-G, possibly

reflecting structural differences between the two seeds. Also, the

levels of contaminating starch and residual protein were high In the

protein and starch fractions respectively. The starch content of the

fines fraction could have been attributable to damaged starch granules

or a population of small starch granules. A different ffillling

procedure may result In Improved Impact milling efficiency.

The use of hulls as a fibre additive may be limited due to

tannins and other toxic constituents In the hull material. Tannin

contents were not quantified In this study but Maris Bead probably had

larger quantities than IVS-G as It has a darker coloured seed coat.

The selection of white seeded varieties may Increase the market

potential of the hull.

Starch concentrates are of less commercial Interest than

protein concentrates. Starch functionality was not studied 1n this

thes1s. However, faba bean starch gelatinization was shown to occur at

a similar temperature to potato and corn starches.

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Isolates, prote1nates and m1cellar proteins had prote1n

contents rang1ng from 83-98%. Equ1valent soy 1solates and prote1nates

have sl1ghtly h1gher prote1n contents. The m1cellar prote1ns were

shown to be the least denatured by DSC analyses. Havever the nat1ve

state of the micellar prote1n was not reflected in 1ts solubility

prof1le. Low values of prote1n solubil1ty were produced at all pH

values. The decreased~H values obta1ned for 1solates and prote1nates

were attr1buted to the effects of isoelectr1c precipltation or prote1n

aggregat1on.

Prote1n functional1ty was assessed in a number of model tests.

The d1fficulties 1n extrapolating from the results obta1ned to real

food systems with many interacting components are s1gn1f1cant.

M1cellar prote1ns d1d not pertorm well 1n any of the funct1onal tests

and this was attr1buted to lack df solubil1ty. However, other stud1es

have demonstrated that m1cellar prote1ns 1n aqueous env1ronments form

f1bres wh1ch can be coagulated by heat. It was suggested that m1cellar

prote1ns may exhiblt desirable funct1onal propert1es in dough type

products. Prote1nates were more soluble and generally exhibited

greater funct1onal1ty than 1solates. 01sulph1de l1nkages formed dur1ng

the storage of isolates were probably respons1ble for the loss of

solub1llty. The presence of pigments m the products caused dark bro.vn

colours to appear at neutral and alkaline pH, or 1n the presence of

salt. The p1gments respons1ble were not 1solated and character1zed but

reports 1n the literature have attr1buted the format1on of coloured

products to phenolic ac1ds. This 1s likely to be a problem m many

food products.

v. faba prote1ns d1d not form f1rm gels even at prote1n

concentrations of 20%. Translucent and sl1ghtly elast1c gels were

tormed at pH values> 7. Globular prote1ns are generally much less

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effect1ve as gell1ng agents than gelat1n or commercially ut1lized

carbohydrate products. However, at h1gh concentrations v. faba

globul1ns may contribute to matrix formation.

Gelling, foaming and emuls1fy1ng properties were largely

dependent on protein concentration. However lipids and fibre d1d

affect performances. Full-fat products had

emuls1fy1ng, but 1nfer1or foam1ng propert1es

1mproved gelling and.

compared to defatted

samples. Isolates and proteinates generally had s1m1lar funct1onal

propert1es to equ1valent soy products. Foaming and emuls1fy1ng

propert1es could probably have been improved by treatment with a

reduc1ng agent. The conduct1v1ty method was considered to give a

better measure of foam qual1 ty.

7S and llS proteins d1d not d1ffer significantly in the1r

behav1our 1n foam1ng or emuls1 fy1ng tests. The small observed

d1fferences were probably caused by m1nor d1fferences in cond1t1ons

dur1ng process1ng. However, the 7S prote1n does undergo a thermal

trans1tion at a lower temperature than the llS prote1n, and they also

exh1b1t d1fferent salt and calc1um ion sens1t1v1t1es. The development

of clon1ng techn1ques to produce large quantit1es of homogeneous

prote1ns, coupled w1th the development of micro-methods w1ll

fac1litate a more comprehens1ve evaluation of these prote1ns.

S1gn1f1cant genet1c variat1on in the llS : 7S prote1n rat1o has been

demonstrated for pea (casey et al., 1982). Furthermore, d1fferent

subun1ts have been shown to contr1bute to varying extents 1n gel

formation. Eventually it may be poss1ble to select spec1f1c variet1es

of legume to match spec1fic funct1onal requ1rements.

In conclusion, V. faba prote1ns and products had s1m1lar

funct1onal propert1es to soy products. Thls 1s not surpr1s1ng

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cons1dering the s1milar1t1es 1n structure. However, the h1gher protein

content of the soy bean enables larger y1elds of protein rich products

to be obtained. The ability of V. faba beans to compete w1th soy beans

will depend on economic factors, and also the development of markets

for the other maJor faba bean constituents, 1e. starch and fibre.

Suggest1ons for further work.

A number of 1ssues were ra1sed in the course of th1s study

wh1ch warrant further research. D1fferences were observed in 1mpact

m1lling effic1ency of Marls Bead and IVS-G seeds. A quant1tat1ve

1solat1on of cell wall mater1al, and SEM of milled flours would help

to elucidate the factors involved in llmiting m1ll1ng eff1c1ency. SEM

of m1lled flours would also g1ve an est1mate of the proportion of

damaged starch granules, and a study of starch part1cle s1ze

distribut1on would indicate whether the contam1nating starch 1n the

prote1n fract1on was due to a populat1on of small starch granules or

damaged starch. If it 1s due to damaged starch granules a change in

the method of mill1ng may improve the separat1on of prote1n and starch

partlcles.

Calcium ions are known to enhance the formation of f1rm gels

from soy prote1ns in the production of tofu. It is l1kely that f1rmer

and more cohesive gels could be produced from V1c1a faba proteins 1n

the presence of calc1um ions.

Flnally, no attempt was made to invest1gate the effects of

chemlcally or physically mod1fy1ng the prote1ns on their funct1onal

propert1es. Mod1ficat1on by the add1t1on of reduc1ng agents, heat

denaturat1on, hydrolysis, acetylat1on and succinylation have been

shown to alter prote1n funct1onality by alter1ng solubility, viscos1ty

and hydrophob1c1ty character1st1cs.

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aiAPI'ER 6

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I would like to thank my family and fr1ends for their encouragement

and support throughout th1s work. I would also like to thank my

colleagues at Durham Un1vers1ty and at the AFRC Institute of Food

Research, Norwich Laboratory, for theu fr1ensh1p and adv1ce.

More spec1f1cally I would l1ke to thank Professor Donald Boulter and

Dr. Dav1d Wr1ght for abta1n1ng financ1al support, and prov1ding

fac1l1t1es for th1s proJect, and for adv1ce and cr1t1c1sm throughout.

Thanks also go to Dr. N1gel Lambert, Mr. John Hemmant and Mr. Timothy

Noel for useful d1scuss1on and pract1cal advice.

I would llke to acknowledge Mr. James Bacon for the DSC thermograms,

and Dr. Mary Parker for the scann1ng electron m1crographs.

Thanks also to Miss Geraldene Slattery and Mr. Trevor Ricketts for

ass1stance with the preparat1on of the manuscr1pt, to M1ss Angela

M1ller for her draw1ng expert1se, and to D.M. Pr1nts for photograph1c

serv1ces.

I acknowledge the rece1pt of a grant from the Sc1ence and Eng1neenng

Research Counc1l.

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