Analysis method of aceclofenac

Description: A white or almost white crystalline powder.
Examine the individual samples by visually.

Reporting: Report as Complies/Does not comply.

Solubility: Freely soluble in acetone, Soluble in ethanol (95 per cent) and Practically insoluble in water.
Procedure: Perform as per GTP
Reporting: Report as Complies/Does not comply.

Identification:
Test A may be omitted if tests B and C are carried out. Tests B and C may be omitted if test A is carried out.

A. By IR.
B. When examined in the range 220nm to 370nm the 0.002% w/v solution in methanol shows an absorption
maximum at 275nm.
C. Dissolve about 10mg in 10ml of ethanol. To 1ml of the solution, add 10.2ml of a mixture of a mixture,
prepared immediately before use, of equal volumes of a 0.6 per cent solution of potassium ferricyanide and a
0.9 per cent solution of ferric chloride. Allow to stand protected from light 5 minutes. Add 3 ml of a 1%
solution of hydrochloric acid. Allow to stand protected from light for 15 minutes. A blue colour develops and
a precipitate is formed.

Reporting: Report as Complies/Does not comply.

Related Substances: < Determine by Liquid Chromatography >

Solvent Mixture: A mixture of 30 volumes of mobile phase A and 70 volumes of mobile phase B.

Test Solution: Dissolve 50mg of the substance under examination in 25ml in solvent mixture.

Reference Solution a: A 0.043 per cent w/v solution of Aceclofenac RS in solvent mixture.

Reference solution b: Dilute 1ml of reference solution a) and 5.0 ml of test solution to 100ml with solvent mixture.

Chromatographic system

– A stainless steel column 25cm x 4.6 mm packed with spherical end-capped octadecylsilane bonded to porous silica (5µm), with a pore size of 10 µm and carbon loading of 19 per cent,
– Mobile phase: A. a 0.112 per cent w/v solution of orthophospheric acid adjusted to pH 7.0 using a 4.2 per cent solution of sodium hydroxide,
B. 1 volume of water and 9 volumes of acetonitrile.
– A linear gradient program using the conditions given below,
– Flow rate. 1ml per minute,
– Spectrophotometer set at 275nm,
– Injection volume: 10µl.

Inject the set solution and reference solution (c). In the chromatogram obtained with the test solution, the area of any secondary peak is not more than 0.2 times the area of the peak in the chromatogram obtained with reference solution (c) (0.2 per cent) and the sum of area of all the secondary peaks is nor more than twice the area of the peak in the chromatogram obtained with the reference solution (c) (0.7 per cent).Ignore any peak with an area less than 0.02 times the area of the principal peak in the chromatogram obtained with reference solution (c) (0.02per cent).

Heavy Metals: 2.0 g complies with limit test for heavy metals, Method B (10 ppm).
Procedure: Perform as per GTP no. SRPL/QC/GTP/005
Reporting: Report as Complies/Does not comply.

Sulphated Ash:
Determined 1.0 gm sample in silica crucible ignite for 800ºC and cool add 1 ml of sulphuric acid or ignite & calculated ash.

Calculation:

% of Ash = Weight of residue x 100

Weight of sample

Reporting: Report in %.

Loss on Drying: Determined on 1g by drying in an oven at 105°.

Calculation:

% of LOD = Loss on weight x 100

Before drying weight

Reporting: Report in %.

Assay:
Weigh accurately about 0.3g and dissolve in 40 ml of methanol. Titrate with 0.1M sodium hydroxide. Determine the end point Potentiometrically .Carry out a blank titration.

1 ml of 0.1M sodium hydroxide is equivalent to 0.03542 g of C16H13Cl2NO4.

Calculation:

Titrate volume x Normality of 0.1M sodium hydroxide x 0.03542 x 100 x 100

0.1 x Spl. wt. x (100-LOD)

Reporting: Report as %.

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