Diclofenac Sodium SR pellets 32% STANDARD ANALYTICAL PROCEDURE
METHOD OF ANALYSIS
1.Description:
Take about 1.0 g of pellets and transfer into suitable clean and dry petri dish spread as evenly in the dish and observe the physical appearance of the pellets. It should be white to off-white in Colour and spherical shaped.
2.Identification By:
UV-Spectrophotometer
The chromatogram obtained by sample preparation corresponds to that of the standard preparation, as obtained in the assay.
3.Loss on Drying:
Take about 1.0 g of the sample and crush it into the powder and determine its loss on drying with the help of LOD apparatus.
It should not more than 5.0%.
4.Sugar Test:
Crush the pellets to powder. Weigh 1gm of sample and transfer it to a beaker. Add 20ml of water and stir it for 10 minutes. Centrifuge it at 6000RPM for 5 minutes. Filter the supernatant.
Dilute 10ml of filtrate to 100ml with D/Water.
To 5ml of the solution add 0.15ml of freshly prepared copper sulphate solution and 2ml of freshly prepared dilute sodium hydroxide (about 1N). The solution is blue and clear and remain so after boiling. To the hot solution add 4ml of dilute HCl (about 1N) and boil for 1 minute. Add 4ml of dilute NaOH solution. No. orange ppt. is formed.
5.Sieve Analysis:
Arrange the sample collector, X1 # sieve, X2 # sieve. Weigh and transfer around 100 gram of the sample into X1 # sieve and shake for 5 minutes. Collect the pellets pass through mesh X1sieve (W X1) and pellets retain on mesh # X2 sieve (W X2).Calculate the % retains and passing as follows
Calculation:
% pass through X1 # mesh W X1 in Gram
= —————————- x 100
weight of sample in Gram
%retain on X2# mesh W X2 in Gram
= ————————— x 100
weight of sample in Gram
6. Gastro Resistance
Acid Release:
- Apparatus: USP apparatus II
- Medium: 0.1 N HCL ,1000 ml
- Sample Interval: 60 minutes
- RPM:75
- Temperature: 37 oC + 0.5 oC
By UV-Spectrophotometer
Sample preparation:
Weigh and transfer the pellets equivalent to 50mg of Diclofenac sodium individually in each of 6 dissolution Baskets, containing 1000ml of 0.1N HCl, equilibrated at 37+ 0.5oC. Immediately start the apparatus and run for 1 hrs. After 1 hour, transfer the acid medium to another set of dissolution baskets and use the intact pellets for Buffer Stage.
To the acid medium add 20ml of 5N NaOH in each of the six dissolution Baskets. Stir it for 5 minutes. After stirring take 20 ml sample and pass it through filter paper.
Dilute 10ml of filtrate to 50ml with 0.1N NaOH .
Reference preparation:
Accurately weigh working reference standard equivalent to 55mg of Diclofenac sodium in a 100ml volumetric flask add 0.1N NaOH to dissolve. Make volume up to mark and sonicate it.
Transfer 1 ml of stock solution to 50 ml volumetric flask and dilute with 0.1 N NaOH to volume and mix.
Procedure:
Take reading of both sample and ref solutions in a 1 cm cell on a U.V/ Visible spectrophotometer at 276 nm using a 0.1 N NaOH as blank.
Calculation:
%age = Absorbance of Sample x conc. of std. solution x 100
Absorbance of standard conc. of smp. solution
Limits: NMT 10% should release after 1 hrs.
7.Dissolution in Buffer
- Apparatus: USP apparatus II
- Medium: Buffer pH = 7.2,1000 ml
- Sample Interval: 3hr and 8hr
- RPM: 75
- Temperature: 37 oC + 0.5 oC
- Weight taken: Equivalent to 55 mg
By UV-spectrophotometer Method
Preparation of Buffer:
3 volume of 0.1N HCl and 1 volume of tri -Sodium Phosphate buffer (0.2M) and adjust to pH 7.2 with either dilute NaOH or dilute Phosphoric Acid.
Reference Preparation:
Accurately weigh working reference standard eq. to 55mg of Diclofenac Sodium and transfer it to a 100ml volumetric flask. Sonicate it to dissolve in 0.1N NaOH. Make volume up to the mark with the same solvent.
Dilute 1 ml of stock solution to 50ml with buffer solution.
Sample Preparation:
After completion of acid stage completely discard 0.1N HCL from each of the 6 dissolution baskets without losing any pellet. Add 1000 ml buffer pH 7.2 to intact pellets in each basket. Run the apparatus for total 8hr (including acid stage) in buffer solution.
Withdraw sample after 2hr of running in Buffer stage(total 3hr) and add equal volume of medium to the dissolution then 8hr of running stop the apparatus. Take 20ml of the sample and pass it through filter paper .take 10ml of the filtrate in 50ml volumetric flask make up to the mark with buffer solution.
Procedure:
Take reading of both sample and ref solutions in a 1 cm cell on a U.V/ Visible spectrophotometer at 276 nm.
Calculation:
%age = Absorbance of Sample x conc. of std. solution x 100
Absorbance of standard conc. of smp. solution
After 3 hrs.: 30% to 65%
After 8 hrs.: NLT 70%.
8. Assay by: UV- spectrophotometer
Standard Preparation:
Accurately weigh working reference standard equivalent to 50mg of Diclofenac sodium in a 100 ml volumetric flask and sonicate it to dissolve in 0.1N NaOH. Make volume up to mark. Dilute 1 ml of stock solution to 50 ml with the same solvent.
Sample Preparation:
Take pellet sample equivalent to 50 mg of Diclofenac sodium to 100 ml volumetric flask. Add 0.1N NaOH to dissolve. Sonicate it for about 30minutes to dissolve. Make volume up to mark with same solvent and stir for about 20-30 minutes. Heat if required.
Centrifuge it at 6000 rpm for 5 minutes (or till a clear supernatant is obtained). Pass it through filter paper. Dilute 1 ml of the filtrate to 50 ml with 0.1N NaOH.
Procedure:
Take reading of both sample and ref solutions in a 1 cm cell on a U.V/ Visible spectrophotometer at 276 nm
Calculation:
%age = Absorbance of Sample x conc. of std. solution x 100
Absorbance of standard conc. of smp. solution
Limits:
28.8% ———35.2% of the label amount
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