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STANDARDISASI

BAHAN ALAM

Kiki Mulkiya Y., M.Si., Apt.

Yani Lukmayani, M.Si., Apt.

Indra T. Maulana, M.Si., Apt.

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KEMURNIAN

KADAR ABU

CEMARAN LOGAM BERAT

CEMARAN MIKROBA

KADAR AIR

PENETAPAN KADAR ABU

Residue on Ignition / Residu Pemijaran

TUJUAN:

Pengujian senyawa anorganik, terutama analisis mineral.

PRINSIP DASAR:

Pemanasan dengan suhu sangat tinggi 450 0C (pemijaran) pada alat tanur

Yang tersisa adalah mineral oksida dan senyawa anorganik

Determination of ash The ash remaining following ignition of herbal materials is

determined by three different methods which measure total ash, acid-insoluble ash and water-soluble ash.

The total ash method is designed to measure the total amount of material remaining after ignition. This include:

physiological ash, which is derived from the plant tissue itself,

non-physiological ash, which is the residue of the extraneous matter (e.g. sand and soil) adhering to the plant surface.

Acid-insoluble ash is the residue obtained after boiling the total ash with dilute hydrochloric acid, and igniting the remaining insoluble matter. This measures the amount of silica present, especially as sand and siliceous earth.

Water-soluble ash is the difference in weight between the total ash and the residue after treatment of the total ash with water.

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Kadar abu total

untuk mengukur jumlah abu total

pada simplisia setelah pembakaran

Logam fisiologis, yg berasal dari jaringan

tanaman itu sendiri (Na, Fe, K,Ca,Mg)

Logam non-fisiologis, yaitu yg merupakan residu benda asing (pasir, tanah)

PROCEDURE

Total ash Place about 24 g of the ground air-dried material,

accurately weighed, in a previously ignited and tared crucible (usually of platinum or silica). Spread the material in an even layer and ignite it by gradually increasing the heat to 500600 C until it is white, indicating the absence of carbon. Cool in a desiccator and weigh. If carbon-free ash cannot be obtained in this manner, cool the crucible and moisten the residue with about 2 ml of water or a saturated solution of ammonium nitrate R. Dry on a water-bath, then on a hot-plate and ignite to constant weight. Allow the residue to cool in a suitable desiccator for 30 minutes, then weigh without delay. Calculate the content of total ash in mg per g of air-dried material.

Kadar abu tidak larut asam

Adalah residu yg tertinggal setelah mendidihkan jumlah abu total dalam HCl

encer, kemudian dibakar lagi

Untuk mengetahui kadar silikat, terutama pasir yg menempel pada simplisia

PROCEDURE (2)

Acid-insoluble ash

To the crucible containing the total ash, add 25 ml of hydrochloric acid (~70 g/l) TS, cover with a watch-glass and boil gently for 5 minutes. Rinse the watch-glass with 5 ml of hot water and add this liquid to the crucible. Collect the insoluble matter on an ashless filter-paper and wash with hot water until the filtrate is neutral. Transfer the filter-paper containing the insoluble matter to the original crucible, dry on a hotplate and ignite to constant weight. Allow the residue to cool in a suitable desiccator for 30 minutes, then weigh without delay. Calculate the content of acid-insoluble ash in mg per g of air-dried material.

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Kadar abu larut air

Adalah perbedaan jumlah abu total dengan residu yg tertinggal setelah dilarutkan dengan

air

Untuk mengetahui logam fisiologis

PROCEDURE (3)

Water-soluble ash

To the crucible containing the total ash, add 25 ml of water and boil for 5 minutes. Collect the insoluble matter in a sintered-glass crucible or on an ashless filterpaper. Wash with hot water and ignite in a crucible for 15 minutes at a temperature not exceeding 450 C. Subtract the weight of this residue in mg from the weight of total ash. Calculate the content of water-soluble ash in mg per g of air-dried material.

Contoh (Suplemen I FHI, 2010)

Buah Cabe Merah:

SIMPLISIA:

Abu Total: Tidak lebih dari 9%

Abu Tidak Larut Asam: Tidak lebih dari 0,1%

EKSTRAK:

Abu Total: Tidak lebih dari 3,4%

Abu Tidak Larut Asam: Tidak lebih dari 0,5%

Akar Kelembak:

SIMPLISIA:

Abu Total: Tidak lebih dari 11,6%

Abu Tidak Larut Asam: Tidak lebih dari 0,5%

EKSTRAK:

Abu Total: Tidak lebih dari 2,3%

Abu Tidak Larut Asam: Tidak lebih dari 0,2%

KEMURNIAN

KADAR ABU

CEMARAN LOGAM BERAT

CEMARAN MIKROBA

KADAR AIR

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Determination of arsenic toxic metals

Arsenic is abundant in nature and its presence in herbal materials should be no different to its wide occurrence in foods.

A popular test method relies on the digestion of the herbal material matrix followed by subjection of the digestate to a comparative colorimetric test in a special apparatus.

The test method described below uses colorimetry and does not use toxic mercuric bromide paper. The method uses N-N-diethylmethyldithiocarbamate in pyridine and it reacts with hydrogen arsenide to afford a redpurple complex. The limit is expressed in terms of arsenic (III) trioxide (As2O3).

Other method: AAS (Atomic Absorption Spectoscopy)

KEMURNIAN

KADAR ABU

CEMARAN LOGAM BERAT

CEMARAN MIKROBA

KADAR AIR

Determination of microorganisms

1. Total viable aerobic count (TVA)/Angka Lempeng Total (ALT)

Prinsip : perhitungan koloni bakteri aerob mesofil setelah cuplikan

diinokulasikan pada media lempeng agar dengan cara tuang, dan

diinkubasi pada suhu yang sesuai. Contoh Media : Plate Count Agar II. Uji Nilai Duga Terdekat (MPN) Coliform

Prinsip : Pertumbuhan bakteri coliform setelah cuplikan diinokulasikan

pada media cair yang sesuai, adanya reaksi fermentasi dan pembentukan

gas di dalam tabung Durham. Contoh Media : Mac Conkey Broth

III. Uji Angka Kapang dan Khamir

Prinsip : Pertumbuhan kapang dan khamir setelah cuplikan

diinokulasikan pada media yang sesuai, diinkubasi pada 20-25C

Contoh Media : Potato Dextrose Agar

IV. Uji Cemaran Aflatoksin

Prinsip : Pemisahan isolat aflatoksin secara Kromatografi Lapis Tipis.

Media dan Pengenceran :Yeast Extract Sucrose Broth (YES)

Tests for specific microorganisms

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Batas Cemaran Mikroba

Berdasarkan WHO:

Penggunaan Mikroba Patogen

Bakteri

/gram

Jamur

/gram

Oral 0 105 103

Topikal 0 107 104

KEMURNIAN

KADAR ABU

CEMARAN LOGAM BERAT

CEMARAN MIKROBA

KADAR AIR

Determination of water

and volatile matter Karl Fischer Titration

Destillation

Gravimetry

Instrumentasi Karl Fischer

Stirrer

Pengukur Potensiometri

Input Air

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[A] Labu Pemanas (Tempat Sampel dan Larutan)

[E] Tube Receiver Distilat Dilengkapi dengan Kran

[C] Tabung Kondensor Refluks

[B] Tabung Konektor Kondensor dengan Receiver [D] Aliran Pipa Penghubung

Labu dengan Sistem Kondensasi

Alat Distilasi Azeotrop Gravimetri

Loss on drying (gravimetric determination)

Place about 25 g of the prepared air-dried material, or the quantity specified in the test procedure for the herbal material concerned, accurately weighed, in a previously dried and tared flat weighing bottle. Dry the sample by one of the following techniques:

in an oven at 100-105 C;

in a desiccator over phosphorus pentoxide R under atmospheric pressure or reduced pressure and at room temperature. Dry until two consecutive weighings do not differ by more than 5 mg, unless otherwise specified in the test procedure. Calculate the loss of weight in mg per g of air-dried material.

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