bovine bone sourcing practices and bone gelatin manufacturing processes in the united states j....

Bovine Bone Sourcing Practices and BoneBovine Bone Sourcing Practices and BoneGelatin Manufacturing ProcessesGelatin Manufacturing Processes

in the United Statesin the United States

J. Michael Dunn, Ph.DVice President, Regulatory Affairs, GELITA North America

Chairman, Regulatory CommitteeGelatin Manufacturers Institute of America (GMIA)

FDA TSE ADVISORY COMMITTEE MEETINGFDA TSE ADVISORY COMMITTEE MEETINGJuly 17, 2003

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US BONE GELATIN MANUFACTURERSUS BONE GELATIN MANUFACTURERS

5%

35%

60%

Photo Pharma Edible

The sourcing practices and processing conditions discussed today will be representative of both US manufacturers

US manufacturers produce primarily limed bone gelatin (Type B) and to some extent acid bone gelatin (Type A)

Eastman Gelatine Corp.Peabody, MA

GELITA USA Inc.Sioux City, IA

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BOVINE BONE SOURCING PRACTICES AND BONE BOVINE BONE SOURCING PRACTICES AND BONE GELATIN MANUFACTURING PROCESSES IN THE USGELATIN MANUFACTURING PROCESSES IN THE US

Overall Objectives Adequately describe the bovine bone sourcing practices

and processing conditions for the manufacturing of bone

gelatin in the US

Confirm that the bone gelatin processing conditions

employed in the US are:

• Virtually the same as those used in the EU

• Meet or exceed all of the minimum processing

requirements as specified in the GME TSE Inactivation

Study Protocol

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BOVINE BONE SOURCING PRACTICESBOVINE BONE SOURCING PRACTICES

Sourcing

Degreased gelatin bone is sourced exclusively from

USDA inspected beef processing facilities in the US

This raw material is derived solely from healthy cattle

that have been deemed fit for human consumption

based upon both ante and postmortem inspections

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BOVINE BONE SOURCING PRACTICESBOVINE BONE SOURCING PRACTICES

SRM’s

All US gelatin bone suppliers have been removing

Specified Risk Materials (SRM’s) with the exception of

vertebrae since as early as 1998

Limited quantities of vertebrae-free gelatin bone have

been available since the Fall of 2002

Currently, there are no FDA or USDA requirements for

the removal of SRM’s in the US

GELATIN MANUFACTURING PROCESS OVERVIEWGELATIN MANUFACTURING PROCESS OVERVIEW

Degreased Gel Bone

HCl Acid Water Labor

Gelatin Process

Dicalcium Phosphate Gelatin

Daily Bone Gelatin Production

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Bone /Type BBone /Type B Bone/Type ABone/Type A

AcidulationAcidulation

Lime TreatmentLime Treatment

WashingWashing

AcidificationAcidification


Acid TreatmentAcid Treatment

WashingWashing

ExtractionExtraction

Initial FiltrationInitial Filtration

Ion ExchangeIon Exchange

Initial ConcentrationInitial Concentration

Final FiltrationFinal Filtration

pH AdjustmentpH Adjustment

Final ConcentrationFinal Concentration

SterilizationSterilization

Chilled ExtrusionChilled Extrusion

DryingDrying

Milling/ScreeningMilling/Screening

BlendingBlending

FormulationFormulation

Final PackagingFinal Packaging

GELATIN MANUFACTURING GELATIN MANUFACTURING PROCESSPROCESS

Overall Objectives Hydrolyze collagen

• Hydrolyze sufficient cross-links and peptide bonds within the collagen matrix to render the hydrolyzed collagen (gelatin) highly soluble in water

Purify the gelatin• Employ appropriate processing steps to ensure

its physical, chemical and microbiological purity Concentrate the finished product

• Use additional processes to remove water from the gelatin liquor to produce a dry, stable product

NaOH OptionNaOH Option

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Typical Characteristics

Fat content = 1 to 2.5%

Size range = 1/8 to 5/8”

Mineral/protein ratio = 1.9 - 2.1

Moisture content = 6 to 9%

In contrast, EU gelatin producers have their own degreasing facilities




WashingWashing



WashingWashing










DryingDrying


BlendingBlending




Incoming Gel BoneIncoming Gel BoneAcid TreatmentAcid Treatment


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Objectives / Conditions

Produce ossein byremoving the mineral content of the bone

Initiate the hydrolysis of collagen Remove non-collagen impurities

HCL concentration: 4-6% Acidulation time: 5-7 days (counter-current

process) Acidulation temperature: 50° to 65° F Washing: Rinse up to 24 hours to remove

acid salts, fat and other impurities




WashingWashing



WashingWashing










DryingDrying


BlendingBlending




AcidulationAcidulationAcid TreatmentAcid Treatment


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Convert asparagine and glutamine to their respective acids (pI decreases)

Lime slurry concentration: Over saturated Lime slurry pH: Approximately 12.5 Liming time: 25-70 days Liming temperature: 50-70° F Agitation: Daily Lime slurry changes: Weekly


Continue to hydrolyze collagen Continue to remove non-

collagen impurities




WashingWashing



WashingWashing










DryingDrying


BlendingBlending




Liming / Type BLiming / Type BAcid TreatmentAcid Treatment


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Remove and neutralize excess lime

Remove non-collagen impurities




WashingWashing



WashingWashing










DryingDrying


BlendingBlending




Washing / AcidificationWashing / Acidification

Adjust pH of the ossein slurry

Wash time: 24 to 48 hours Agitation: Vigorous Water temperature: 45° to 70° F Neutralizing acids: Hydrochloric & sulfuric Target pH: 5 to 7



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Objective / Conditions

Condition ossein for extraction at low pH

Traditional• Treatment: Sulfuric acid at pH = 1.0 - 2.0• Treatment time: = 6 hours• Washing: Rinse up to 24 hours to a pH of

2.8 - 3.2 Alkaline pre-treatment option (under review)

• pH is maintained at 13 or greater with NaOH for 3 hours (prior to acid treatment)




WashingWashing



WashingWashing










DryingDrying


BlendingBlending




Acid Treatment / Type AAcid Treatment / Type A

>



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending




Gelatin ExtractionGelatin Extraction


Solubilize hydrolyzed collagen (gelatin) from the ossein

Water purity: Demineralized Procedure: Series of extractions with

increasing water temperatures Water temperatures: 120° to 200° F Conditioning time: 1 to 6 hours / extraction Number of extractions: 4 to 6



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending






Clarify dilute gelatin solution Protect ion exchange system

Vertical leaf pressure filter Pre-coated with diatomaceous earth and

cellulose Gelatin concentration: 4-6%



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending






Deionize the thin gelatin liquor

Cations removed: Ca+2, Mg+2 and Fe+2

Anions removed: Cl- or S04=

Ash (product): 0.1 to 1%



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending






Concentrate the thin gelatin liquor

Evaporator type: Multiple effect rising film or plate and frame

Concentration target: 15-25% Output temperature: 115° F to 150° F



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending






Clarify concentrated gelatin solution

Remove additional coagulated protein and particulate

Plate and flame pressure filters Cellulose / diatomaceous earth filter pads



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending






Fine adjustment of the finished product pH

Final pH targets: 5-7 Caustic adjustment: NaOH



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending






Concentrate the thick gelatin liquor

Evaporator type: Thin film / wiped surface or plate and frame multiple effect

Output temperature: 115° to 125° F Concentration target: 25 to 50% (viscosity dependent)



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending






Ensure microbiological purity / product hygiene

Equipment: Direct steam injection / HTST Temperature: 138° to 149° C Time: 8 to 16 seconds



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending






Increase the surface area of the gel mass

Glycol - cooled heat exchanger / extruder Temperature: Approx. 70° F Noodle dimensions: 1’ to 2’ long / 1/8” thick



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending




DryingDrying


Produce a dry, stable product

Air quality: Heated, dehumidified and filtered Number of zones: 10 to 12 Temperature gradient: 80° to 160° F Time: 1 - 3 hours Moisture content (gelatin): 10 to 12%



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending




Milling and ScreeningMilling and Screening


Grind gelatin to a uniform size

Equipment: Cage mill Particle size: 8 to 30 mesh



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending




BlendingBlending

Blender

Drummingand

weighing

QC/QA Analysis



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending





Component Selection

High Capacity Blender

QC/QA Analysis



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WashingWashing



WashingWashing










DryingDrying


BlendingBlending





Drums

FIBCs

Small Bags



bovine bone sourcing practices and bone gelatin manufacturing processes in the united states j....

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