standard testing procedure diclofenac sodium

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:

25 g

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

Quantity of Control Sample:

2 X 25 g

Description: A white to slightly yellowish crystalline powder; slightly hygroscopic.

Solubility: Freely soluble in methanol; soluble in ethanol (95 per cent); sparingly soluble in water and in glacial acetic acid; practically insoluble in ether, in chloroform and in toluene.

Identification:

Test A may be omitted if tests B, C, and D are carried out. Tests B and C may be omitted if tests A and D are carried out

A. By IR.
B. A dark red colour develops.
C. The principal peak in the chromatogram obtained with the test solution corresponds to the peak in
The chromatogram obtained with the reference solution.
D. A 1.0 per cent w/v solution gives the reaction of sodium salts.

Appearance of solution: Not more intensely coloured than reference solution BYS6.

pH: 6.5 to 8.5

Light Absorption: Absorption at about 440nm NMT 0.050.

Related Substances: In the chromatogram obtained with the test solution; the area of any peak is not greater than the area of the principal peak is not greater than the area of the principal peak in the chromatogram obtained with the reference solution (0.2 per cent); the sum of the areas of all peaks other than the principal peak is not greater than 2.5 times that of the principal peak in the chromatogram obtained with the reference solution (0.5 per cent). Ignore any peak with an area less than 0.25 times the area of the principal peak in the chromatogram obtained with the reference solution.

Heavy Metals: NMT 10ppm.

Loss on drying: NMT 0.5%w/w.

Assay: 98.5% to 101.0%w/w on the dried basis.

Description: A white to slightly yellowish crystalline powder; slightly hygroscopic.

Solubility: Freely soluble in methanol
Soluble in ethanol (95 per cent)
Sparingly soluble in water and in glacial acetic acid
Practically insoluble in ether, in chloroform and in toluene.

Identification:

Test A may be omitted if tests B, C, and D are carried out. Tests B and C may be omitted if tests A and D are carried out

A. By IR.
B. To 1ml of a 0.4 per cent w/v solution in methanol add 1ml of nitric acid; a dark red colour develops.
C. In the test for related substances, the principal peak in the chromatogram obtained with the test solution corresponds to the peak in the chromatogram obtained with the reference solution.
D. A 1.0 per cent w/v solution gives the reaction of sodium salts.

Appearance of solution:
A 5.0 per cent w/v solution in methanol is clear and not more intensely coloured than reference solution BYS6.

pH: 6.5 to 8.5, deter mined on a 1.0 per cent w/v solution.

Light Absorption: Absorbance of a 5.0 per cent w/v solution in methanol at about 440nm, not more than 0.050.

Related Substances: Determine by liquid chromatography

Test solution: Dissolve 50mg of the substance under examination in methanol and dilute to 50ml with the same solvent.

Reference solution: A 0.0002 per cent w/v solution of diclofenac sodium RS in methanol.

Chromatographic system

– a stainless steel column 25cm X 4.6mm, packed with end-capped octylsilane bonded to porous silica (5µm),
– Mobile phase: a mixture of 34 volumes of a solution containing 0.5g per liter of phosphoric acid and 0.8g per liter of sodium dihydroen phosphate adjust to pH 2.5 with phosphoric acid, and 66 volumes of methanol.
– Flow rate. 1ml per minute,
– spectrophotometer set at 254nm,
– Injection volume. 20µl.

Inject the test solution and the reference solution. In the chromatogram obtained with the test solution: the area of any peak other than the principal peak is not greater than the area of the principal peak in the chromatogram obtained with the reference solution (0.2 per cent); the sum of the areas of all peaks other than the principal peak is not grater than 2.5 times that of the principal peak in the chromatogram obtained with the reference solution (0.5 per cent). Ignore any peak with an area less than 0.25 times the area of the principal peak in the chromatogram with reference solution.

Heavy Metals: 1.0 g complies with the limit test for heavy metals, Method B (10ppm).

Loss on drying: Not more than 0.5 per cent, determined on 1.0 g by drying in an oven at 105° for 3 hours.