standard testing procedure dextromethorphan hydrobromide

Storage Requirements:
Store protected from light and moisture.
Sampling:
Sample equal quantity from each container / bag. Collect a minimum of 5g from each container/bag sample into individual, self –sealing clear polythene bag kept in another clear self sealing polythene bag bearing ‘Sample for Analysis,lable.After completion of sampling return rest sample on same container. Collect control sample in Pet Bottle/Glass Bottle.
Quantity of Composite Sample:
15 g
Quantity of individual Identification
0.0100 g from each container /bag.
Quantity of Control Sample:
2 X 15 g

Description: An almost white crystalline powder.
Solubility: Freely soluble in ethanol (95 per cent) and in chloroform; sparingly soluble in water; practically
Insoluble in ether.

Identification

:
Test A may be omitted if tests B, C and D are carried out. Tests B and C may be omitted if tests A and D are carried out.
A. By IR: Determine by infrared absorption spectrophotometer. Compare the spectrum with that obtained with
Dextromethorphan HBr RS.
B. An absorption maximum only at about 278nm.
C. In the test for related substances, the principal peak in the chromatogram obtained with test solution corresponds to that in the chromatogram obtained with reference solution.
D. Gives the reaction of bromides.
Appearance of solution: clear and colourless.
Acidity or alkalinity: The solution is yellow and not more than 0.4ml of 0.01M hydrochloric acid is required to change the colour to red.
Specific optical rotation: +28.0° to +30.0
N,N-Dimethylaniline: The resulting solution is not more intensely coloured than that obtained by treating at the same time and in the same manner a solution containing 5µg of N, N-dimethylaniline in 20ml of water.
Related Substances: Determine by liquid chromatography
I) Single Maximum Impurity: NMT – 0.5%.
II) Any other Impurity: NMT – 0.25%.
III) Total Impurity: NMT – 1.0%.
Sulphated Ash: NMT 0.1%w/w.
Water: 4.0% to 5.5%w/w.
Assay: 99.0% to 101.0%w/w on anhydrous basis.

Description: An almost white crystalline powder.
Reporting: Report as Complies/Does not comply.
Solubility: Freely soluble in ethanol (95 per cent) and in chloroform, sparingly soluble in water, practically insoluble in ether.
Reporting: Report as Complies/Does not comply.
Identification:
Test A may be omitted if tests B, C and D are carried out. Tests B and C may be omitted if tests A and D are carried out.
A. By IR: Determine by infrared absorption spectrophotometer. Compare the spectrum with that obtained with Dextromethorphan HBr RS.
B. When examined in the range 230nm to 360nm, a 0.01 per cent w/v solution in 0.1M hydrochloric acid shows an absorption maximum only at about 278nm.
C. In the test for related substances, the principal peak in the chromatogram obtained with test solution corresponds to that in the chromatogram obtained with reference solution.
D. Gives the reaction of bromides.

Reporting: Report as Complies/Does not comply.
Appearance of solution: A 5.0 per cent w/v solution in ethanol (95 per cent) is clear and colourless.
Reporting: Report as Complies/Does not comply.
Acidity or alkalinity: Dissolve0.4gm in carbon dioxide-free water with gentle heat, cool and dilute to 20ml with same solvent. Add 0.1ml of methyl red solution and 0.2ml of 0.01M sodium hydroxide. The solution is yellow and not more than 0.4ml of 0.01M hydrochloric acid is required to change the colour to red.
Reporting: Report as Complies/Does not comply.
Specific optical rotation: Determined in a 2.0 per cent w/v solution in 0.1 M hydrochloric acid.

Reporting: Report as value in º.
N,N-Dimethylaniline: Dissolve 0.5g in 20ml water with the help of gentle heat on a water-bath, cool and add 2ml of 2M acetic acid, 1 ml of a 1 per cent w/v solution of sodium nitrite and sufficient water to produce 25 ml. The resulting solution is not more intensely coloured than that obtained by treating at the same time and in the same manner a solution containing 5µg of N, N-dimethylaniline in 20ml of water.
Reporting: Report as Complies / D
oes not comply.

Related Substances: Determine by liquid chromatography
Test Solution: Dissolve 10mg of the substance under examination in 10.0ml of the mobile phase.
Reference solution (a): A 0.0005 % w/v solution of dextromethorphan hydrobromide RS in the mobile phase. (Dissolve 50mg of the Dextromethorphan Hydrobromide RS in 100.0ml of the mobile phase. Take 1.0ml of this solution and dilute to 100ml with mobile phase).
Reference solution (a1): Precede same as reference solution (a).
Chromatographic system
– a stainless steel column 25cm x 4.6 mm packed with octadecylsilane bonded to porous silica (5µm),
– mobile phase: dissolve 3.11g of docusate sodium in a mixture of 400 ml of water and 600 ml of acetonitrile, Add 0.56g of ammonium nitrate, adjust the pH to 2.0 with glacial acetic acid,
– Flow rate. 1ml per minute
– spectrophotometer set at 280 nm
– Injection volume. 20µl.
Inject the test solution and the reference solution. Run the chromatogram twice the retention time of the principal peak. In the chromatogram obtained with the test solution the area of any secondary peak is not more than the area of the principal peak in the chromatogram obtained with reference solution (0.5per cent). The area of one such peak is not more than 0.5 times the area of the principal peak in the chromatogram obtain with reference solution.(0.25 per cent), and sum of all other secondary peaks is not more than twice the area of the principal peak in the chromatogram obtained with reference solution (1.0 per cent). Ignore any peak with an area less than 0.1 times the area of the principal peak in the chromatogram obtained with the reference solution .(0.05 per cent).

System suitability requirement:

3] The column efficiency for the peak of Dextromethorphan Hydrobromide obtained in the chromatogram of individual
reference Solution (a) injected in replicates (including bracketing standard ) and reference solution (a) is not less then
2000 theoretical plates. (Report the value obtained from the fist injection of replicate of reference Solution (a) as well as
last bracketing standard).
Sulphated Ash: Weight accurately 1.0gm of sample in silica crucible ignites in muffle farness at 700ºC for 120 minutes.

Revision No.	Changes
00	First Time Prepare
01	Periodic Revision and Review of Formating Standard Testing Procedure & Formate
02	Periodic Revision and Review of Formating Standard Testing Procedure & Formate
03	Periodic Revision change

standard testing procedure dextromethorphan hydrobromide

Leave a Comment Cancel reply