QUALITY CONTROL
Document code: Issue status: Effective date:
Page 1 of 5
QC/SOP-002 01 06-03-2016
DOCUMENT TITLE:
STANDARD ANALYTICAL PROCEDURE
FOR
ALUSIM SUSPENSION
PURPOSE & SCOPE:
It is established for chemical analysis of ALUSIM SUSPENSION (Bulk and filled bottles) and is applicable to Quality Control
department.
RESPONSIBILITY:
1. Manager Quality Control.
2. Assistant Manager Quality Control
3. .Quality Control Analyst.
Each 5ml Contains:
Aluminium Hydroxide USP ……………….. 215mg
Magnesium Hydroxide USP ………………… 80mg
Simethicone USP ……………………………… 25mg
Product Spec: USP
2. DESCRIPTION:
2.1 Description: Milky white suspension having characteristic aroma of pine apple.
3. TESTS:
3.1 Identification:
a. Magnesium: Mix 5 ml with 10 ml of 2M hydrochloric acid, add 5 drops of methyl red
solution and heat to boiling. Add 6M ammonia until the solution becomes yellow;
continue boiling for 2 minutes and filter. To 1 ml of the filtrate add 1 ml of 6M
ammonia and 1 ml of 2M ammonium chloride; no precipitate is produced. Add
0.25M disodium hydrogen orthophosphate; a white, crystalline precipitate is
produced which is insoluble in 6M ammonia.
b. Aluminium: Wash the precipitate obtained in Identification test for Magnesium with
hot ammonium chloride solution (1 in 50), and dissolve the precipitate in
hydrochloric acid. Divide this solution into two portions: the dropwise addition of
6N ammonium hydroxide to one portion yields a gelatinous white precipitate,
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QUALITY CONTROL
Document code: Issue status: Effective date:
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QC/SOP-002 01 06-03-2016
DOCUMENT TITLE:
STANDARD ANALYTICAL PROCEDURE
FOR
ALUSIM SUSPENSION
which does not dissolve in an excess of 6N ammonium hydroxide. The dropwise
addition of 1N sodium hydroxide to the other portion yields a gelatinous white
precipitate, which dissolves in an excess of 1N sodium hydroxide, leaving some
turbidity.
c. Simethicone: Perform the identification test on infra-red spectrometer using the
standard and sample solutions prepared for assay of simethicone.
3.2 pH: 7.0 to 8.6.
4. ASSAY:
Assay of Aluminium Hydroxide:
Assay preparation: Measure the weight per ml of suspension and transfer weight of Oral
Suspension, previously well-shaken in its original container, equivalent to about 1000 mg of
aluminum hydroxide, to a 250ml beaker. Add 20 ml of water, stir, and slowly add 10 ml of
hydrochloric acid. Heat gently, if necessary, to aid solution, cool, and filter into a 250ml
volumetric flask. Wash the filter with water into the flask, add water to volume, and mix.
Procedure: Pipet 10 ml of the Assay preparation into a 250-ml beaker, add 20 ml of water, then
add, in the order named and with continuous stirring, 25.0 ml of Edetate disodium titrant
(0.05M) and 20 ml of acetic acid- ammonium acetate buffer TS, and heat near the boiling
temperature for 5 minutes. Cool, add 50 ml of alcohol and 2 ml of dithizone TS, and mix.
Titrate with 0.05 M zinc sulfate VS until the color changes from green violet to rose-pink.
Perform a blank determination, substituting 10 ml of water for the Assay preparation, and
making any necessary correction. Each ml of 0.05 M Edetate disodium titrant consumed is
equivalent to 3.900 mg of Al(OH)3.
(VB - VS) x F x 3.9 x 250 x 5 x D
Percent Content = x 100
W x 10 x 215
Percent Content
Found Amount = x 215
100
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QUALITY CONTROL
Document code: Issue status: Effective date:
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QC/SOP-002 01 06-03-2016
DOCUMENT TITLE:
STANDARD ANALYTICAL PROCEDURE
FOR
ALUSIM SUSPENSION
where;
VB = Volume of 0.05M Zinc sulfate used for blank determination.
VS = Volume of 0.05M Zinc sulfate used for un-reacted EDTA.
F = Molarity Factor of Zinc sulfate solution.
W = Weight of sample taken for assay preparation (in grams).
D = Weight per ml of suspension (g/ml).
Limit: 90.0 ~ 110.0 %
Assay of Magnesium Hydroxide:
Assay Preparation: Use the solution prepared for assay preparation of aluminium.
Procedure: Pipet 25ml of the Assay preparation into a 400-ml beaker, add 200 ml of water and
20 ml of triethanolamine, and stir. Add 10 ml of ammonia-ammonium chloride buffer TS and 3
drops of an eriochrome black indicator solution prepared by dissolving 200 mg of eriochrome
black T in a mixture of 15 ml of triethanolamine and 5 ml of dehydrated alcohol, and mix. Cool
the solution to between 3° and 4° by immersion of the beaker in an ice bath, then remove, and
titrate with 0.05M edetate disodium VS to a blue endpoint. Perform a blank determination,
substituting water for the Assay preparation, and make any necessary correction. Each ml of
0.05 M Edetate disodium consumed is equivalent to 2.916 mg of Mg(OH) 2.
Volume of 0.05M EDTA used for sample (VEDTA) after blank correction = VS - VB
VEDTA x F x 2.916 x 250 x 5 x D x 100
Percent Content = W x 25 x 80
Percent Content
Found Amount = 100 x 80
where;
VB = Volume of 0.05M EDTA used for blank determination.
VS = Volume of 0.05M EDTA used for sample.
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QUALITY CONTROL
Document code: Issue status: Effective date:
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QC/SOP-002 01 06-03-2016
DOCUMENT TITLE:
STANDARD ANALYTICAL PROCEDURE
FOR
ALUSIM SUSPENSION
VEDTA = Volume of 0.05M EDTA used for sample after blank correction.
F = Molarity Factor of EDTA solution.
W = Weight of sample taken for assay preparation (in grams).
D = Weight per ml of suspension (g/ml).
Limit: 90.0 ~ 110.0 %
Assay of Simethicone:
Sample Preparation: Transfer an accurately measured volume of Oral Suspension, equivalent
to about 50 mg of simethicone, to a suitable round, narrow-mouth, screw-capped, 120-ml
bottle, add 40 ml of 0.1 N sodium hydroxide, and swirl to disperse. Add 25.0 ml of toluene,
close the bottle securely with a cap having an inert liner, and shake for 15 minutes, accurately
timed, on a reciprocating shaker (e.g., about 200 oscillations per minute and a stroke of 38 ± 2
mm). Transfer the mixture to a 125-ml separator. Remove about 5 ml of the upper, organic
layer to a screw-capped, 15-ml test tube containing 0.5 g of anhydrous sodium sulfate. Close
the tube with a screw-cap having an inert liner, agitate vigorously, and centrifuge the mixture
until a clear supernatant liquid (Assay preparation) is obtained.
Standard Preparation: Prepare a Standard preparation similarly, except to dissolve about 50
mg of Polydimethylsiloxane reference standard, accurately weighed, in 25.0 ml of toluene, add
40ml of 0.1N sodium hydroxide, and add a volume of water equal to that of the specimen of
Oral Suspension taken.
Blank Preparation: Prepare a blank by mixing 10 ml of toluene with 0.5 g of anhydrous
sodium sulfate and centrifuging to obtain a clear supernatant liquid.
Concomitantly determine the absorbances of the solutions in 0.5-mm cells at the wavelength of
maximum absorbance at about 7.9 µm, with an infrared spectrophotometer, using the blank to
set the instrument. Calculate the result as following:
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QUALITY CONTROL
Document code: Issue status: Effective date:
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QC/SOP-002 01 06-03-2016
DOCUMENT TITLE:
STANDARD ANALYTICAL PROCEDURE
FOR
ALUSIM SUSPENSION
where;
As = Absorbance of sample solution.
Ar = Absorbance of standard solution.
Wr = Weight of standard (in mg).
Ws = Weight of sample (in gram).
D = Weight per ml (gram per ml).
P = Percentage Purity of standard.
Limit: 85.0 ~ 115.0 %
4.
5. \
6.
COMPOSITION:
RELATED DOCUMENTS
S.No Document Title Document Code S.No Document Title Document Code
1 Request for Analysis QF/PRD/002 5 “Approved” slip QF/QC/008
2 Product Entry Register QF/QC/005 6 “Adjust” slip QF/QC/012
Analysis Certificate for finished
3 Analysis Record for Products QF/QC/016 7 QF/QC/013
product.
4 Q.C Analysis Certificate for ------- QF/QC/004
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