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Cyclobenzaprine HCl SR Pellets Testing Procedure

Cyclobenzaprine HCl SR Pellets Testing Procedure

Description:

Take about 1.0 g of pellets and transfer it to a clean and dry petridish spread evenly in the dish and observe the physical a appearance of the pellets. It should be pale yellow to creamy colored.

Identification By: HPLC

The retention time of the major peak in the chromatogram of the sample preparation corresponds to that of the standard preparation, as obtained in the assay.

Identification By: UV-Spectrophotometer

The spectrum obtained by sample preparation corresponds to that of the standard preparation, as obtained in the assay.

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%.

Sugar Test

Crush the pellets to powder. Weigh 1 gm 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.

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 X2sieve (W x2) and pellets retain on mesh# X1 sieve (W x1).Calculate the% retains and passing as follows

Calculation:

Dissolution

  • Apparatus: USP apparatus II
  • Medium: 0.1 N HCL ,900 ml
  • Sample: Interval 02, 04, 08 and 16 hrs
  • RPM: 50
  • Temperature: 37 °C ± 0.5°C

Sample preparation:

Weigh and transfer the pellets equivalent to 50mg of Cyclobenzaprine HCl, individually in each of 6 dissolution baskets, containing 900 ml of 0.1 N HCl, equilibrated at 37± 0.5°C. Immediately start the apparatus and run for 16 hrs. After 2 hours lift the paddle and take 20 ml of the sample. Filter it and use the filtrate.
After withdrawal, add 20ml of 0.1 N HCl to each dissolution basket and keep running the apparatus.
Repeat the same process after 4 hrs., 8hrs of dissolution and then finally take the sample after l 6hrs.
Each time dilute 10ml of filtrate to 50ml with 0.1 N HCl.

Reference preparation:

Transfer 10mg of Cyclobenzaprine-HCl working standard, accurately weighed, to a 100 ml volumetric flask. Add 0.1 N HCl as solvent and sonicate for about 15 minutes to dissolve. Make volume up to mark.
Dilute 5ml of the solution to 50 ml with the same solvent.

Procedure

Take reading of both sample and ref solutions in a 1 cm cell on a U.V/ Visible spectrophotometer at 290 nn1, using 0.lN HCl as blank

Calculation: 

Limits:
After 2hrs: NMT40%
After 4 hrs: 43%-63%
After 8 hrs: 66%-86%
After 16 hrs: NLT 80%

Assay
a)By HPLC

Chromatographic conditions

  • Column: 4.6mm x 150 cm; 5 µm packing L1
  • Wavelength: 290nm
  • Flow rate: 1.5 ml/minute
  • Injection volume: 20 µl
  • Buffer: Add 3.7 ml of methane sulfonic acid per 1 L of water and adjust with diethylamine to a pH of 3.6
  • Mobile phase: Acetonitrile, methanol and buffer (25.5:21.0:53.5)
  • Diluent: Acetonitrile and water (50:50)

Standard preparation: 0.12 mg/ml of USP Cyclobenzaprine-HCl RS in diluent
Sample preparation: Crush the pellets to powdered form .Take sample equivalent to 60 mg and transfer to 100 ml volumetric flask. Add 80 ml of diluent and stir for about 30 -40 minutes. Make volume up to mark and sonicate for about 30 -40 minutes. Centrifuge and filter .Take 10 ml of filtrate to 50 ml volumetric flask and make up to mark with diluent.
(0.12mg/ml of Cyclobenzaprine-HCl)

Calculation:

b)UV-Spectrophotometer (Alternate IH Method)
Standard Preparation

Take Cyclobenzaprine-HCl working standard equivalent to 50 mg, accurately weighed, in a 100 ml volumetric flask. Add 0.1 N HCl and sonicate for about 15-20 minutes to dissolve. Make volume up to mark with the same solvent.
Dilute I ml of the solution to 50 ml with the same solvent.

Assay Preparation

Crush the pellets to powdered form. Weigh accurately powdered sample equivalent to 50 mg of Cyclobenzaprine HCl and transfer it to a 100 ml volumetric flask. Use 0.1 N HCl as a solvent. Carry out a sonication process for 20-30 minutes, along with heating at 80°C. Then stir it for 20-30 minutes. Again sonicate for about 30 minutes. Then cool it to room temperature and make volume up to mark with 0.1 N HCl.(Due to extended release nature, it will take a little longer time for drug release.)
Filter and dilute 1 ml of the filtrate to 50 ml with 0.1 N HCl.

Procedure

Take reading of both sample and ref solutions in a l cm cell on a U.V/ Visible spectrophotometer at 290 nm.

Calculation:

Limits: 90% – 110% of the labeled Amount

 

 

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