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SUKRASNO SITI KUSMARDIYANI

Physical and Chemical Parameters of Crude Drugs and Their Products

PART 1

Geneva, 9-13 October 1978 A “ Meeting on selection and characterization of medicinal plants (vegetable drugs)”

Suggested that “In view of the current importance ofand interest in vegetable drugs, it is necessary to preparean international Codex containing general control methodsand specific monograph on such drugs”.

1. Microscopical and histochemical techniques for the morphological analysis of the drugs, whole or in powder form

2. Techniques for determination of loss on drying and water content

3. Techniques for the determination of extractable substances, essential oils or ash

4. Tests to determine the presence of undesirable substances (adulterants, pesticides, preservatives, etc.)

5. Any other general test required, particularly the test for purity (freedom from microorganisms and parasites)

General Control Methods

1. USP United States Pharmacopoeia XIX, 19752. BP British Pharmacopoeia 19733. EuP European Pharmacopoeia I-1969, II-1971, III-1975,

Supplement to Volume II-1973, to Volume III- 19774. SSRP State Pharmacopoeia of the Union of Soviet Socialist Republics, X,

1968 (in Russian)5. ChP Pharmacopoeia of the People’s Republic of China, 1978 (in Chinese)6. JP The Pharmacopoeia of Japan, IX (English edition), 19767. IndP Pharmacopoeia of India, I, 19558. IP The International Pharmacopoeia III, I (1951, 55, 59), II (1967)9. PhFr. Pharmacopée Française, IX, 1972

10. PhHelv. Pharmacopoeia Helvetica, VI, 197111. PhIt. Farmacopea Ufficiale della Repubblica Italiana, VIII, 197212. PhDDR Arzneibuch der Deutschen Demokratischen Republik, II, 197513. Ph Hung. Pharmacopoea Hungarica, VI (English edition), 1970

The Pharmacopoeias Consulted

Lou, Z., 1980, General Control Method for Vegetable Drugs, Comparative Study of Methods Included in Thirteen Pharmacopoeias and Proposals on Their International Unification.

1. General notices2. Powder fineness and sieve size3. General advise on sampling4. Determination of foreign matter5. Macroscopic and microscopic examination6. Thin–layer chromatography7. Determination of ash8. Determination of extractable matter9. Determination of water and volatile matter

10. Determination of volatile oils

Chapters to be discussed:

Topics 5, 7, 8, 9, and 10 will be more elaborated as part of laboratory activities.

“dry to constant weight”

“precision”

- General notices -

“solubility”

Describe these commonly used terms:

WHO, 1998, Quality Control Methods for Medicinal Plant Materials.

“storage condition”

In a refrigerator

Cold or cool

Room temperature

… – … oC

…. – … oC

… – … oC

- General notices -

Find other terms and explain.

- Microscopic examination -

Clarification of microscopic particles

Chloral hydrate

Calcium carbonate

Calcium oxalate


Andrographidis herba

Cannabis herba

© SK

© SK

Ver. 22SK005

+ HCl

+ HCl

Explain

©KUSMARDIYANI

ERGASTIC CELL CONTENT

Trease, 537.

Calcium oxalate crystals

A-D tetragonal systemE-I monoclinic system

A1-A3 Rosette crystals of tetragonal system

D a tetragonal prismE a monoclinic prismG raphidesH a single needle crystalI a sphaerocrystal


Rheum officinale Baillon.Polygonaceae

RHEI RADIX

Source: root and rhizome of Rheum officinale Baillon, R. palmatum L., other species of Rheum except R. rhaponticum L.

Rhubarb, Rheum, Chinese rhubarb, Kelembak

Rein-8-glukosida

Tyler, 64

© KUSMARDIYANI

AKAR KELEMBAK

Ver. 22SK005

MMI IV, 231-233.

SERBUK AKAR KELEMBAK

PENAMPANG MELINTANG AKAR KELEMBAK

RHEI RADIX

Stahl, 89.

RHEI RADIX

Rhei radix© KUSMARDIYANI

Ver. 22SK005

Write microscopic information of this pulverized crude drug.

Alstonia scholaris R. Br. Apocynaceae

ALSTONIAE CORTEX

© SK

Ver.22SK005

KULIT BATANG PULE

© SK

Alstonia scholaris R. Br.Apocynaceae

© KUSMARDIYANI

MMI IV, 3 - 5.

ALSTONIAE CORTEX

ALSTONIAE CORTEX

Tombol pengatur halus mikroskop diputar sehingga dapat terfokuskan pada daerah bawah medan pengamatan.

Kristal kalsium oksalat yang sebagian berbentukmonoklinik, karena pembiasan cahaya dan penggeseranfokus pengamatan pada saat tombol halus diputar, akanterlihat seperti “buku atau jendela terbuka”.

Ver. 22SK005

“flour and starch”

Explain the differences:

How much should be collected from each container ?

• Crude drug has specific characters, i.e.: low homogeneity, and need specific sampling method.

Sampling of Crude Drug

Sample Collection

Microscopic Particle Size

• Microscope• Ocular Micrometer• Objective Micrometer

Equipments:

Steps of Measurement

1. Calibrate ocular micrometer with objective micrometer2. Measurement of particle

Calibration:• Ex. :100 scales of ocular superimposed with 30 scale

of objective micrometer. • 100 scale = 30 x 0,01 mm• 1 scale = 3 µm


Alignment of the stage micrometer and the ocular micrometer

Definition of foreign matter• Parts of medicinal plant material or material other

than those named with limits scpecified for the plant material concerned.

• Any organism, part of an organism, other than that named in the specification and description of the plant material concerned.

• Mineral admixtures not adhering to the medicinal plants materials, such as soil, stones, sand, and dust.

Determination of Foreign Matter

Sample size• Roots, rhizomes, and barks 500 g• Leaves, flowers, seeds, and fruits 250 g• Cut medicinal plants

with average weight of fragment < 0.5 g 50 g

Recommended procedures• Spread the sample and collect foreign matter

• Sift the remainder through sieve no 250, and the dust mineral admixture.

• For foreign matter similar to the crude drug, critical test that base on physical and chemical tests may be needed.

Water Content and Lost on Drying

• Water content is the water present in the crude drug.

• Lost on drying is the decrease of crude drug weight on drying at 105oC.

• Compounds evaporate at 105oC is not only water.

• Lost on drying is the rapid method to estimate water content.

Water Content Determination

Azeotrop DistillationWater forms azeotrop mixture with toluene or xylene, evaporate together and separate following condensation. The distillate is collected in scaled tube.

The Saturation of Toluene• Toulene is mixed with water and distilled until the

volume of water in the distillate remain constant.

• Toluene is shaken with water and the excess of water separated.

EuPPhDDR

USP & ChP

SSRP

Apparatus for the determination of water by azeotropic distillation

Differences:-Capacity of distilling flask-Length of condenser-Length of vertical portion of connecting tube-Receiving tube-Distilling liquid-Quantity of sample taken-Anti-bumping material-Distillation rate


Apparatus for the determination of water content by azeotropic method

WHO, 1998, Quality Control Methods for Medicinal Plant Materials

dimensions in mm

Learn more about the method!

Apparatus to determine water content by distillation methodinMATERIA MEDIKA INDONESIA

Compare with method and apparatus recommended by the WHO

KARL FISHER TITRATION

• Not suitable for crude drug• Suitable for extract

Explain!!

BP

PhDDR

SSRP Method 2

SSRP Method 1

Apparatus for the determination of volatile oils in vegetable drugs

Differences:- Weight of sample- Distillation liquid- Capacity of flask - Rate of distillation- Volume of xylene added- Duration of distillation- Capacity & subdivision of

measuring tube



measuring tube


JP PhHelv in mm

ChP in cm

Apparatus for the determination of volatile oils in vegetable drugs


measuring tube


EuP Apparatus for the determination of volatile oils in vegetable drugs

Apparatus to determine volatile oils


dimensions in mm

Apparatus to determine volatile oil contentinMATERIA MEDIKA INDONESIA

Compare with the method and apparatus recommended by the WHO

Macroscopic and Microscopic Examination

Macroscopic inspection:shape, size, colour, surface characteristic, texture, fracture characteristic, appearance of the cut surface

Microscopic inspection:preparation of specimen, treatment using chemical reagents,characteristic fragments,types of stomata & stomatal index,etc.

Take appropriate notes from this textbook.

Use forceps to separate each component of the mixture. There are 12 crude drugs. Now write common name for each of these crude drugs!

The answers can be seen on the next slide.

© KUSMARDIYANI

Now write Latin name for each of these crude drugs.

If you don’t know the right answers, go the next slide.

Bunga kenanga

Bunga cengkeh

Daun sirih

Rimpang laos

Rimpang kunir

Daun kemuning

Kulit batang lemo

Buah ketumbar

Buah pinang

Biji kopi

Daun jambu biji

Daun jati belanda

© KUSMARDIYANI

Canangii flos

Caryophylli flos

Piperis betle folium

Languatis rhizoma

Curcumae domesticae rhizomae

Murrayae folium

Litseae cortex

Coriandri fructus

Arecae semen

Coffeae semen

Psidii folium

Guazumae folium

© KUSMARDIYANI

Try once again to mention Latin name for each of these medicinal plant materials.

1

2

3

4

5

6 7

8

9

10

11

© KUSMARDIYANI

It seems that you can only get 11 items unless you make them separated before identifying each of these crude drugs

Languatis rhizoma

© KUSMARDIYANI

If you still have difficulties, try to start again from the first slide.

Canangii flos

Piperis albi fructus

Psidii folium

Guazumae folium

Curcumae domesticae rhizoma Murrayae folium

Piperis betle folium

Arecae semen

Coffeae semen

Litseae cortex

MICROSCOPIC EXAMINATION A mixture of 4 powdered crude drugs

© KUSMARDIYANI

Ver. 22SK005The mixture was observed using chloral hydrate solution

Arecae semenArtemisiae herba Curcumae domesticae

© KUSMARDIYANI

Ver. 22SK005

This powdered crude drug was observed using chloral hydrate solution

How to identify the starch? Another preparation using water (+ glycerin) is needed. -- Explain --

Amylum solaniCurcumae domesticae rhizoma

© KUSMARDIYANI

Ver. 22SK005

The same mixture was observed using water (+ glycerin)

How do you identify that these starches come from different sources? Explain.

Write Latin name of the 4 crude drugs in this mixture. The answers are on the next slide.

© KUSMARDIYANI

Ver. 22SK005

Powdered crude drug was observed using chloral hydrate solution

Sappan lignumPsidii folium

Parkiae semen

Theae foliumTry to obtain the characteristic fragments

by moving to other parts of the slide.

© KUSMARDIYANI

Ver. 22SK005

Give complete descriptions of these characteristic fragments.

LABORATORY OF PHARMACOGNOSY - SCHOOL OF PHARMACY - INSTITUT TEKNOLOGI BANDUNG

More examples of crude drug examination can be learned from:

- Kusmardiyani, School of Pharmacy ITB -

1. General notices2. Powder fineness and sieve size3. General advise on sampling4. Determination of foreign matter5. Macroscopic and microscopic examination6. Thin–layer chromatography7. Determination of ash8. Determination of extractable matter9. Determination of water and volatile matter

10. Determination of volatile oils

We have discussed several basic concepts and significant points of their application. Do the best you can to summarize each chapter below and explain each step of the recommended procedures.

WHO, 1998 (2005), Quality Control Methods for Medicinal Plant Materials.

------Check your notes soon after class and briefly review the notes before the next class-----

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