## STP FOR ACECLOFENAC TABLETS

1.0) Description: Visual

2.0) Average Weight: Check weight of 20 tablets at randomly and calculate the average weight by formula :  wt of 20 tablets (gm) x 1000                                              / 20. found avg. wt in mg

3.0)  Uniformity of weight:

Weigh 20 tablets selected at random and calculate the average weight. Not more than two of the individual weights deviate from the average weight by more than the percentage shown in table.

Tablets were weighed individually and the percentage of deviation of its weight from the average weight was determined for each tablet. Formula for calculate the percentage of deviation = (experimental weight – theoretical weight)    x 100%

Theoretical weight

 Average weight of tablets Percentage deviation More than 80mg but Less than 250mg 7.5% 250mg or More 5%

4.0)      Identification Test:

In the Assay, the principal peak in the chromatogram obtained with the test solution corresponds to the peak in the chromatogram obtained with the reference solution.

5.0)      Hardness:

The standard method used for tablet hardness testing is compression testing. The tablet is placed between two jaws that crush the tablet. The machine measures the force applied to the tablet and detects when it fractures. Although compressive force is applied to the tablet, along the diameter of the tablet at right angles to the applied force.

6.0)      Disintegration Time

Unless otherwise stated in the individual monograph, introduce one tablet into each tube and add a disc to each tube. The assembly is suspended in the liquid medium in a suitable vessel, preferably a 1-litre beaker. The volume of liquid is such that the wire mesh at its highest point is at least 15mm below the surface of the liquid, and at its lower point is at least 25mm above the bottom of the beaker. At no time should the top of the basket-rack assembly become submerged. There is a thermostatic arrangement for heating the liquid and maintaining the temperature at 37±2°.

If 1 or 2 tablets fail to disintegrate, repeat the test on 12 additional tablets; not less than 16 of the total of 18 tablets tested disintegrate.

If the tablets adhere to the disc and the preparation under examination fails to comply, repeat the test omitting the disc. The preparation complies with the test if all the tablets in the repeat test disintegrate.

7.0)      Dimension of Tablet:

Length, breadth and thickness are determined by vernier in mm

8.0)      Dissolution:

Medium: 900ml of phosphate buffer pH 7.5

Time: 45 minutes

Speed: 50 rpm

Limit: NLT 75% of the stated amount of Aceclofenac.

Withdraw a suitable volume of the medium and filter. Reject the first few ml of the filtrate and dilute a suitable volume of the filtrate with dissolution medium. Measure the absorbance of the resulting solution at the maximum at about 273nm. Calculate the content of Aceclofenac in the medium from the absorbance obtained from a solution of known concentration of Aceclofenac reference standard in the same medium.

9.0)      Leak test:

The apparatus is used to test for the integrity of packed strips, blisters and Alu-Alu Blister pack containing tablets. Ensure apparatus bath is filled with purified water upto mark indicated and add 0.5% crystal violet solution in water. Samples are placed into the desiccators and the lid is placed in position. The pump starts to produce a vacuum 15inHg inside the desiccators and the vacuum is held for 1 minute. The sample remains at the required vacuum level for given time interval buzzer will sound after time is over and will cut off the vacuum pump. As the package is immersed in a colored dye solution the venting of the desiccators will allow any holes to be penetrated by the dye and the contents of the flexible packaging will also be stained with the same coloring material.

Examine all the strips for any leakage by opening the pockets manually. If anyone pocket shows evidence of leakage, reject the sample, stop the Blister / Strip machine and immediately take corrective action.

10.0)    Related substance: Determined by liquid chromatography.

Solvent mixture: 50 volumes of acetonitrile and 50 volumes of water.

Test solution: Disperse a quantity of powdered tablets containing 100mg of aceclofenac  with the solvent mixture anddilute to 100.0ml with the solvent mixture, filter.

Reference solution (a): A 0.1 per cent w/v solution of aceclofenac reference standard in the solvent mixture.

Reference solution (b): Dissolve a quantity of diclofenac sodium reference standard containing 25mg of diclofenac in the solvent mixture and dilute to 25.0ml with the solvent mixture. Dilute 1.0 ml of this solution and 1.0 ml of reference standard (a) to 100.0ml with the solvent mixture.

Chromatographic system:

• A stainless steel column 25cmX4.6mm packed with dimethyloctylsilane bonded to porous silica (5µm) (such as Hypersil MOS),
• Mobile phase: a mixture of 55 volumes of buffer pH 3.5 prepared by adding 1.2ml of glacial acetic acid in 1000ml of water, adjusting the pH to 3.5 with dilute sodium hydroxide solution, 22.5 volumes of acetonitrile and 22.5 volumes of tetrahydrofuran,
• Flow rate: 1ml per minute,
• Spectrophotometer set at 275nm,
• Injection volume: 20µl

Inject reference solution (b). The test is not valid unless the resolution between the peaks due to aceclofenac and diclofenac is not less than 5.0 and the column efficiency is not less than 2000 theoretical plates for peak due to aceclofenac.

Inject reference solution (b) and the test solution. In the chromatogram obtained with the test solution, the area of peak due to diclofenac is not more than 5 times the area of the peak due to diclofenac in the chromatogram obtained with reference solution (b) (5.0 per cent). The area of any other secondary peak is not more than the area of the principal peak in the chromatogram obtained with reference solution (b) (1.0 per cent) and the sum of the areas of all the secondary peaks other than diclofenac peak is not more than twice the area of the peak in the chromatogram obtained with the reference solution (b) (2.0 per cent).

11.0)    Assay: Determined by liquid chromatography.

Solvent mixture: 55 volumes of acetonitrile and 45 volumes of water.

Test solution: Weigh and powder 20 tablets. Disperse a quantity of powder containing 100mg of aceclofenac with 60 ml of acetonitrile, with the aid of ultrasound for 10 minutes and dilute to 100.0ml with acetonitrile. Dilute 5.0ml of this solution to 50.0ml with the solvent mixture.

Reference solution: A 0.1 per cent w/v solution of aceclofenac reference standard in acetonitrile. Dilute 5.0ml of this solution to 50.0ml with the solvent mixture.

Chromatographic system:

• A staianless steel column 15cmX4.6mm packed with octadecylsilane bonded to porous silica (5µm), (such as Hypersil ODS)
• Mobile phase: a mixture of 55 volumes of buffer solution prepared by adding 1.0ml of G.A.A. in 1000ml of water and 45 volumes of acetonitrile.
• Flow rate: 1.5ml per minute,
• Spectrophotometer set at 275nm,
• Injection volume: 20µl

Inject reference solution. The test is not valid unless the column efficiency is not less than 2500 theoretical plates, the tailing factor is not more than 2.0 and the relative standard deviation for replicate injections is not more than 2.0 per cent.

Inject reference solution and the test solution.

Calculate the content of Aceclofenac in the tablet.

Formula  for calculation:

Area of test     Weight of STD        5           100               50       Potency

—————-X——————–X——X—————-X——-X——–XAverage wt.

Area of STD              100              50     Weight of test     5         100

Alternative Method: By UV Spectrophotometer

Test Solution: Weigh and powder 20 tablets. Weight sample equivalent to 50mg of Aceclofenac 100ml volumetric flask add 20ml methanol into it and sonicate to dissolve the test sample. Make up to mark with methanol. Filter and dilute 2ml of this solution to 50ml in same 0.1 M HCl.

Reference Solution: Weigh 50mg of reference standard of Aceclofenac in 100ml of volumetric flask. Add 20ml methanonl into it and sonicate to dissolve. Dilute 2ml of this solution to 50ml with 0.1 M HCl.

Check Absorbance of test as well as reference standard at about 275nm in UV Spectrophotometer.

Calculate the content of Aceclofenac in the tablets.

Formula:

Area of Test      STD Wt.(mg)  2            100               50       Potency

—————–X————–X——-X—————X——–X———–X Average wt.

Area of STD        100              50      Test Wt.(mg)     2           100

Acceptance criteria: 90.0%-110.0%

12.0)    MICROBIOLOGICAL PURITY

Perform the test according to requirements of IP,

Total aerobic Microbial count (TAMC): NMT 103 CFU/g

Total combined yeasts/Moulds count (TYMC): NMT 102 CFU/g

Pathogens: in 1gm drug.

Escherichia Coli – Should be absent

Pseudomonas aeroginosa – Should be absent

Salmonella – Should be absent

Staphylococcus aureus– Should be absent

Abbreviations:

Wt.: Weight

mg: Miligram

ml: Milileter

STD: Standard

inHg: Inch of Mercury

rpm: Rounds per minute

CFU: Colony forming unit

OPA: Orthophosphoric acid

G.A.A: Glacial acetic acid