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Department : Quality Control Department Title : Aceclofenac IP Name of Mfg. / Suppliers : Total Qty. Recd.: Batch No: Testing Date : Sr. Test No. 01 Description 02 Solubility Result

Raw Material Test Protocol Page No : 01 of 04 Sample Qty. : A.R. No : Completion Date: Specification A white or almost white, crystalline powder. Practically insoluble in water, freely soluble in acetone, soluble in ethanol (95 % ).

03 04 05 06 07 08

Identification Related substance Heavy metals Loss on drying Sulphated Ash Assay

(A)By IR spectrophotometry (B)

NMT 0.5% NMT 0.1% 99% to 101%

Report : In the opinion of the undersigned , the sample refered to above is COMPLIES / NOT COMPLIES standard quality as IP/ SPECIFICATION.

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Department : Quality Control Department Title : Aceclofenac IP

Raw Material Test Protocol Page No : 02 of 04

1. Description: A white or almost white, crystalline powder. Complies / Does Not Complies 2.Solubility: Practically insoluble in water, freely soluble in acetone, soluble in ethanol (95 % ). Complies / Does Not Complies Identification Test A may be omitted if tests B and C are carried out. test B & C may be omitted if test A is carried out. A: determine by infrared absorption spectrophotometry (2.4.6.) APPARATUS: An infrared spectrophotometer for recording the spectra in the infrared region consist of an optical system of providing the monochromatic light in the region of 4000 cm-1 to 625 cm-1 ( about 2.5 m to 16 m ) and the means of measuring the quotient of intensity of the transmitted light and theincident light . Fourier transform infrared spectrophotomrters that are replacing the conventional dispersive instruments use polychromatic radiation and calculate the spectrum in the frequency domain from the original data by Fourier transformation. For recording the infrared spectra , the instrument should comply with the following test for resolution. Control of resolution performance: for instrument having a monochromator , record the spectrum of a polystyrene film approximately 35 m in thickness. The difference x between the percentage transmittance at the transmission maximum A at 2870 cm-1 (3.48 m ) and that at the transmission maximum B at 2849.5 c m-1 (3.51 m ) must be greater than 18 . The difference y between the percentage transmittance at the transmission maximum C at 1589 cm-1 (6.29 m ) and that at the transmission minimum D at 1583 cm-1 (6.32 m ) must be greater than 10. For fourier transform instruments, use suitable instrument resolution with the appropriate apodisation prescribed by the manufacturer. The resolution is checked by the suitable means, for example by recording the spectrum of polystyrene film approximately 35 m in thickness . The difference between the absorbances at the absorption minimum at 2870 cm-1 absorption maximum at 2849.5 cm-1 is greater than 0.33.The difference between the absorbances at the absorption minium at 1589 cm-1 and absorption maximum at 1583 cm-1 is greater than 0.08. Verification of the wave number scale: the wave number scale may be verified using polystyrene film, which has transmission minima ( absorption maxima) at the wavw numbers ( in cm-1) shown in the table 1.

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Table 1 : transmission minima and acceptable tolerances of a polystyrene film ________________________________________________________________ Transmission Acceptable tolerance ( cm-1)________ Minima ( cm-1) Monochromator Fourier-transform Instruments instruments ______________________________________________________________ 3060.0 2849.5 1942.9 1601.2 1583.0 1154.0 1028.3 1.5 2.0 1.5 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0

______________________________________________________________ PREPARATION OF SAMPLE: A sample of the substance under examination may be prepared in one of the following ways. (a) For normal recording : liquids- examine a liquid as a thin film held between two plates or in a cell of suitable path-length constructed of material transplant to infrared radiation in the region to be examined. Liquids or solids to prepared as solutions prepare a solution in a suitable solvent and use a concentration and path-length to give a satisfactory spectrum over a sufficiently wide wavelength range.Absorption due to solvent should be compensated for by placing in the reference beam a similar cell containing the solvent used; it should be noted that absorption bands due to the substance under examination that coincide with strong solvent absorption will not be recorded. Suitable concentrations of the solute will very with the substance being examined but typical concentrations are 1 % to 10 % at 0.5 to 0.1 mm path- length. Solids- examine a solid after dispersion in a suitable liquid ( mull ) or solid ( potassium halide disc ), as appropriate. Mulls- triturate 1 to 5 mg of the substance with the minimum amount of liquid paraffin or other suitable liquid to give a smooth creamy paste. Compress a portion of the mull between two suitable plates. Discs- triturate about 1 mg of the substance with approximately 300 mg of dry , finely powdered potassium bromide IR or potassium chloride IR, as directed. These quantities are usually suitable for a disc 13 mm in diameter. Grind the mixture thoroughly , spread it uniformly in a suitable dia and compress under vaccum at a pressure of about 800 MPa. Commercial dies are available and the manufacturer s instruction should be strictly followed . Mount the resultant disc in a suitable holder in the Analysis by: Date: Checked by: Date: Approved by: Date:

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spectrophotometer. Several factors , such as inadequate or excessive grinding , moisture or other impurities in the halide carrier, may give rise to unsatisfactory discs. A disc should be rejected , if visual inspection shows lack of uniformity or if the transmittance at about 2000 cm-1 ( 5 m ) in the absence of the specific absorption band is less than 75 % without compensation. If the other ingredients of tablets, injections, and other dosage forms are not completely removed from the substance being examined , they may contribute to the spectrum. (b) for recording by the multiple reflection :when directed in the individual monograph, prepare the sample by one of the following methods solutions- dissolve the substance in the appropriate solvent under the conditions described in the individual monograph . Evaporate the solution on a thallium bromo-iodide plate or any other suitable plate. Solids- place a substance on a thallium bromo-iodide plate or any other suitable plate in a manner giving uniform contact. Identification by reference substances- unless otherwise directed in the individual monograph, prepare the substance under examination and the reference substance in the form of disc dispersed in the potassium bromide IR or potassium chloride IR and record the spectra between the 4000 cm-1 and 625 cm-1 ( 2.5 m to 16 m ) under the same operational conditions. The absorption maxima in the spectrum obtained with the substance under examination correspond in position and relative intensity to those in the spectrum obtained with the reference substance . When the spectra recorded in the solid state show differences in the positions of the absorption maxima , treat the substance under the examination and the reference substance in the same manner so that they crystallise

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B. Dissolve 50.0 mg in methanol R and dilute to 100.0 ml with the same solvent. Dilute 2.0 ml of the solution to 50.0 ml with methanol R. Examined between 220 nm and 370 nm (2.2.25), the solution shows an absorption maximum at 275 nm. The specific absorbance at the absorption maximum is 320 to 350. Complies / Does Not Complies C. Dissolve about 10 mg in 10 ml of alcohol R. To 1 ml of the solution, add 0.2 ml of a mixture, prepared immediately before use, of equal volumes of a 6 g/l solution of potassium ferricyanide R and a 9 g/l solution of ferric chloride R. Allow to stand protected from light for 5 min. Add 3 ml of a 10.0 g/l solution of hydrochloric acid R. Allow to stand protected from light for 15 min. A blue colour develops and a precipitate is formed. Complies / Does Not Complies Related substances: Complies / Does Not Complies Heavy metals: Maximum 10 ppm. To 2.0 g in a silica crucible, add 2 ml of Sulphuric acid R to wet the substance. Heat progressively to ignition and continue heating until an almost white or at most a greyish residue is obtained. Carry out the ignition at a temperature not exceeding 800 C. Allow to cool. Add 3 ml of hydrochloric acid R and 1 ml of nitric acid R. Heat and evaporate slowly to dryness. Cool and add 1 ml of a 100 g/l solution of hydrochloric acid R and 10.0 ml of distilled water R. Neutralize with a 1.0 g/l solution of ammonia R using 0.1 ml of phenolphthalein solution R as indicator. Add 2.0 ml of a 60 g/l solution of anhydrous acetic acid R and dilute to 20 ml with distilled water R. 12 ml of the solution complies with limit test A. Prepare the standard using lead standard solution (1 ppm Pb) R. Complies / Does Not Complies Analysis by: Date: Checked by: Date: Approved by: Date:

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Department : Quality Control Department Title : Aceclofenac IP

Raw Material Test Protocol Page No : 03 of 04

Loss on drying : Maximum 0.5 per cent, determined on 1.000 g by drying in an oven at 100-105 C. Before Drying Wt. of LOD Bottle: Wt. of Crusible + Subs: Wt. of Substance: Calculation: % of LOD = Wt. of Loss X 100 / Taken Subs. % of LOD = x 100 / = % Complies / Does Not Complies Sulphated ash: Maximum 0.1 per cent, determined on 1.0 g. Before Ignition Wt. of Crucible: Wt. of Crucible + Subs: Wt. of Substance: Calculation: % of Ash = Wt. of Ash X 100 / Taken Subs. % of Ash = x 100 / = % Complies / Does Not Complies Gm Gm Gm After Ignition Wt. of Crucible : Wt. of Crucible + Ash: Wt. of Ash: Gm Gm Gm Gm Gm Gm After Drying Wt. of LOD Bottle : Wt. of Bottle + LOD: Wt. of LOD: Gm Gm Gm

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Department : Quality Control Department Title : Aceclofenac IP ASSAY

Raw Material Test Protocol Page No : 04 of 04

Dissolve 0.300 g in 40 ml of methanol R. Titrate with 0.1 M sodium hydroxide, determining the end-point potentiometrically. 1 ml of 0.1 M sodium hydroxide is equivalent to 35.42 mg of C16H13Cl2NO4. Taken Substance : B.R : ml of gm M Sodium hydroxide

Calculation : B.R X Normality X Factor x 100 0.1 X Taken Subs. X = % Complies / Does Not Complies X 0.03542 x 100 0.1 X Taken Subs.

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