3/3/2014

KEMURNIAN
KADAR ABU

STANDARDISASI
BAHAN ALAM

CEMARAN LOGAM BERAT

CEMARAN MIKROBA

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

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

KADAR AIR
1

PENETAPAN KADAR ABU

Residue on Ignition / Residu Pemijaran
TUJUAN:

Pengujian senyawa anorganik, terutama analisis

mineral.

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:

PRINSIP DASAR:
Pemanasan dengan suhu sangat tinggi 450 0C
(pemijaran) pada alat tanur
Yang tersisa adalah mineral oksida dan senyawa
anorganik

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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PROCEDURE
Total ash
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)

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.

PROCEDURE (2)

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

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 acidinsoluble ash in mg per g of air-dried material.

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PROCEDURE (3)

Kadar abu larut air

Adalah perbedaan jumlah abu total dengan
residu yg tertinggal setelah dilarutkan dengan
air
Untuk mengetahui logam fisiologis

Contoh (Suplemen I FHI, 2010)

Buah Cabe Merah:

SIMPLISIA:
Abu Total: Tidak lebih dari 9%
Abu Tidak Larut Asam: Tidak
lebih dari 0,1%

Akar Kelembak:
SIMPLISIA:
Abu Total: Tidak lebih dari 11,6%
Abu Tidak Larut Asam: Tidak
lebih dari 0,5%

EKSTRAK:
EKSTRAK:
Abu Total: Tidak lebih dari 3,4% Abu Total: Tidak lebih dari 2,3%
Abu Tidak Larut Asam: Tidak
Abu Tidak Larut Asam: Tidak
lebih dari 0,5%
lebih dari 0,2%

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 sinteredglass 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.

KEMURNIAN
KADAR ABU
CEMARAN LOGAM BERAT
CEMARAN MIKROBA
KADAR AIR

3/3/2014

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)

Determination of microorganisms

KEMURNIAN
KADAR ABU
CEMARAN LOGAM BERAT
CEMARAN MIKROBA
KADAR AIR

Tests for specific 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)

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KEMURNIAN

Batas Cemaran Mikroba

Berdasarkan WHO:

Penggunaan Mikroba
Patogen

Bakteri
/gram

Jamur
/gram

Oral

105

103

Topikal

107

104

KADAR ABU
CEMARAN LOGAM BERAT
CEMARAN MIKROBA
KADAR AIR

Determination of water
and volatile matter

Karl Fischer Titration

Destillation

Gravimetry

Instrumentasi Karl Fischer

Input Air
Stirrer
Pengukur Potensiometri

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Alat Distilasi Azeotrop

Gravimetri

[C] Tabung Kondensor Refluks

[B] Tabung Konektor

Kondensor dengan Receiver

[E] Tube Receiver Distilat

Dilengkapi dengan Kran

[D] Aliran Pipa Penghubung

Labu dengan Sistem Kondensasi

[A] Labu Pemanas

(Tempat Sampel dan Larutan)

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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