Standard testing procedure mefenamic acid

Storage Requirements:
Store protected from light and moisture.

Sampling:
Sample equal quantity from each container / bag. Collect a minimum of 5g from each container/bag sample into individual, self –sealing clear polythene bag kept in another clear self sealing polythene bag bearing ‘Sample for Analysis,lable.After completion of sampling return rest sample on same container. Collect control sample in Pet Bottle/Glass Bottle.
Quantity of Composite Sample:

15 g

Quantity of individual Identification
0.0100 g from each and every container /bag.

Quantity of Control Sample:

2 X 15 g

Description: A white to greyish-white, microcrystalline powder; odourless or almost odourless.

Solubility: Sparingly soluble in ether; slightly soluble in ethanol (95per cent) and in chloroform; practically insoluble in water.

Identification:

A. By IR.
B. Absorbance at 365nm
C. An intense blue colour is produced immediately which fades rapidly to brownish-green.

Light absorption: Maximum at about 279nm and 350nm,

Copper: NMT 20ppm

Related Substances: Any secondary spot in the chromatogram obtained with the test solution is not more intense than the spot in the chromatogram obtained with the reference solution.

2, 3 Dimethylaniline: Determine by Thin Layer chromatography
Any spot corresponding to 2, 3 dimethylaniline in the chromatogram obtained with the test solution is not more intense than the spot in the chromatogram obtained with the reference solution.

Sulphated Ash: NMT 0.1 %w/w.

Loss on drying: NMT 1.0 %w/w.

Assay: 99.0% to 100.5%w/w on the dried basis.

Description: A white to greyish-white, microcrystalline powder; odourless or almost odourless.

Solubility: Sparingly soluble in ether
Slightly soluble in ethanol (95per cent) and in chloroform
Practically insoluble in water.

Identification:

A. By IR.
B. Dissolve 25mg in 15ml of chloroform and examine in ultraviolet light at 365nm; the solution
exhibits a strong greenish –yellow fluorescence. Carefully add 0.5ml of a saturated solution of
trichloroacetic acid drop wise and examine again in ultraviolet at 365nm; the solution does not
exhibit fluorescence.
C. Dissolve 5mg in 2ml of sulphuric acid and add 0.05ml of 0.0167 M potassium dichromate; an intense blue colour is produced immediately which fades rapidly to brownish – green.

Light absorption:
Absorbance of a 0.002 per cent w/v solution in a mixture of 99 volumes of methanol and 1volume of 1M hydrochloric acid at the maximum at about 279nm, 0.69 to 0.74 and at maximum at about 350nm, 0.56 to 0.60.

Copper:
Moisten 1.0g with sulphuric acid and ignite until all the carbon is removed, Add 10ml of 1M sulphuric acid to the residue and allow to stand for 10 minutes.

Transfer to a separating funnel using 20ml of water and add 10ml o f a solution containing 20 per cent w/v diammonium hydrogen citrate and 5
percent w/v solution of disodium edetate. Add 0.2ml of thymol blue solution and neutralize with 5M ammonia. Add 10ml of sodium diethyldithiocarbonate solution and 15ml of carbon tetrachloride, shake and allow to separate. The yellow colour of the carbon tetrachloride layer is not more intense than that produced by treating 2ml of copper standard solution (10ppm Cu) in the same manner beginning at the words” Transfer to a separating funnel using …” (20 ppm).

Related Substances: Determine by Thin layer chromatography

Solvent mixture: 3 volumes of chloroform and 1 volumes of toluene, 25 volumes of dioxin and 1 volume of glacial acetic acid.
Mobile phase: A mixture of 90 volumes of toluene, 25 volumes of dioxin and volume of glacial acetic acid.
Test solution: Dissolve 0.25g of the substance under examination in 10ml of the solvent mixture.
Reference solution: Dissolve 5.0 mg of the substance under examination in 100ml of the solvent mixture. Apply to the plate 20µl of each solution. After development dry the p[late in air, expose to iodine vapour for 5minutes and examine in UV light at 254nm. Any secondary spot in the chromatogram obtained with the test solution is not more intense than the spot in the chromatogram obtained with the reference solution.

2, 3-Dimethylaniline: Determine by Thin layer chromatography

Solvent mixture: 3 volumes of chloroform and 1 volume of methanol.

Mobile phase: A mixture of 90 volumes of toluene, 25 volumes of dioxin and 1volumes of 18M ammonia.

Test solution: Dissolve 0.25g of the substance under examination in 10ml of the solvent mixture

Reference solution: A 0.00025 per cent w/v solution of 2, 3-dimethylaniline in the solvent mixture.

Apply to the plate 40µl of each solution. After development, dry the plate in a current of warm air. Spray the plate with ethanolic sulphuric acid (20 per cent), heat at 105°C for 30 minutes and immediately expose to nitrous fumes may be glass chamber for 15 minutes (the nitrous fumes may be generated by adding dilute sulphuric acid drop wise to a solution containing 10 per cent w/v sodium nitrite and 3 per cent w/v of potassium iodide) . If necessary, allow to dry and repeat the praying. Any spot corresponding to 2, 3 –dimethylaniline in the chromatogram obtained with the test solution is not more intense than the spot in the chromatogram obtained with the reference solution.

Assay:
Weigh accurately about 0.5g and dissolve in 100ml of warm ethanol (95 per cent) previously neutralized to phenol red solution and titrate with 0.1 M sodium hydroxide using phenol red solution as indicator.

1ml of 0.1M sodium hydroxide is equivalent to 0.02413g of C15H15NO2.

DOCUMENT CHANGE HISTORY

Revision No.	Changes
00	First Time Prepare
01	Periodic Revision and Review of Formating Standard Testing Procedure & Formate
02	Periodic Revision and Review of Formating Standard Testing Procedure & Formate
03	Periodic Revision change