Analysis method of Dried Aluminium Hydroxide Magnesium Hydroxide Oxetacaine and Simethicone suspension

1.0 OBJECTIVE
1.1 To lay down a procedure for analysis of Dried Aluminium Hydroxide, Magnesium Hydroxide, Oxetacaine &Simethicone Suspension.

2.0 SCOPE
2.1 This procedure is applicable to the analysis of Dried Aluminium Hydroxide, Magnesium Hydroxide, Oxetacaine and Simethicone Suspension.in Quality control

3.0 RESPONSIBILITY
3.1 Q.C- Chemist

4.0 ACCOUNTABILITY
4.1 Manager-Quality Assurance

5.0 Procedure

5.1 Description: Pour 50 ml finish sample in beaker and observed visually.

5.2 pH: Taken 50 ml sample in beaker rinse the pH electrode first with purified water followed by sample dip the electrode in sample and observed the pH.

5.3 Volume variation: Measured the volume by measuring cylinder and determine the volume variation.

5.4 Identification:
5.4.1 In the assay, the principle peak in the chromatogram obtain with the test solution correspond to the peak in the chromatogram obtained with the reference solution. and by chemical method.
5.5 ASSAY:
Each 5ml contains:
Dried Aluminium Hydroxide I.P 600mg./ 250mg.
Magnesium Hydroxide I.P 300mg./ 250mg.
Simethicone I.P 25mg./ 25mg.
Oxetacaine B.P 10mg./ 10mg.

Method of Dried Aluminium Hydroxide, Magnesium Hydroxide, Oxetacaine &Simethicone suspension.
Estimation of Dried Aluminium Hydroxide.
By Titration:
Taken 3.0 gm. or 5.0gm. as per sample weight added 3ml of concentrated hydrochloride acid, dilute to 100ml with water, warmed on water bath and cooled. To 20ml of the above sample solution, add 80ml water and 40ml 0.05 M disodium edetate. Neutralized by the dropwise addition of 1M sodium hydroxide using methyl red solution as indicator. Warm on a water bath for 30 minutes, add 3 gm hexamine and titrate with 0.05 lead nitrate, using xylenol orange solution as indicator. Each ml of 0.05 M disodium edetate is equivalent to 0.002549g of aluminum oxide. (Al2O3)

V= Volume (in ml) of Lead Nitrate. Solution consumed in titration.

N = Actual normality of Lead Nitrate Solution.

AW= Average weight

Wt. = Weight of Sample.

Calculation:

Estimation of Magnesium Hydroxide.

To 25ml of sample as prepared under examination of Aluminium Hydroxide. Add 25 ml of Triethanolamine and 10 ml of Ammonia Ammonium Chloride Buffer solution. Titrate with 0.05 m E.D.T.A using erichrome black T indicator
Each ml of 0.05 M E.D.T.A is equivalent to 0.002916 of magnesium hydroxide.

Ammonia Ammonium chloride buffer:

6.75 gm Ammonium Chloride add 20 ml water and 57 ml of Ammonia produced to 100 ml water.

V= Volume (in ml) of E.D.T.A. Solution consumed in titration.

N = Actual normality of E.D.T.A Solution.

AW= Average weight.

Wt. = Weight of Sample.

Calculation:

Estimated of Simethicone:
ASSAY:
Transferred an Accurately equivalent 50 mg of Simethicone in 25 ml of dilute hydrochloric acid extract with four 40 ml of petroleum ether (40 to 600c). wash the organic layer with tow 10 ml. portion of water, filter the organic layer through anhydrous sodium Sulphate, collect the filter in pre-dried weighed beaker and dry it on a water Bath and then in air oven at 1050c for one hour.
The difference in weight is the amount of simethicone present in the weight quantity of the sample taken for analysis.

Estimation of Oxetacaine
BY HPLC
Buffer: 0.136 gm of potassium di hydrogen orthophosphate buffer was taken diluted to 1000ml with water. adjusted to pH. 3.5 with Orthophosphate.

Mobile phase: Acetonitrile: Buffer
30 : 70

Solvent mixture: Acetonitrile: water
50 : 50

Standard preparation: Weight accurately about 20mg Oxetacaine. Diluted to 100 ml volumetric flask with solvent mixture.
Sample preparation: Taken Accurately equivalent to 20 mg of sample weight. Diluted to 100 ml volumetric flask with solvent mixture.
Chromatographic condition:
Wavelength -214nm
Flow rate – 1.0 ml /mint.
Column -C18 (150 x4.6) 5µm
Injection volume – 20µl
Temperature – 250c
Retention time -About 2.75 mint.

Calculation:

6.0 Abbreviation

Sr. No.	Abbreviation used	Full form of abbreviation used
1.0	STP	Standard Testing Procedure
2.0	QA	Quality assurance
3.0	STD	Standard
4.0	SPL	Sample
5.0	NM	Nano Meter