Dextromethorphan Hydrobromide Raw Material Testing specification & analysis prescribes the requirements with IR spectrum and Alternate Method of Analysis on UV System and Other Testing procedures.
Dextromethorphan Hydrobromide Raw Material Testing PURPOSE
This raw material specification & analysis prescribes the requirements Dextromethorphan Hydrobromide Raw Material Testing which is used in Syrup & Tablet.
1.0 PURPOSE
This raw material specification & analysis prescribes the requirements for Dextromethorphan Hydrobromide which is one of the components of Syrup & Tablet.
2.0 SCOPE
It is applicable in Material Department, Product Development and Quality Assurance Department to confirm its physical and chemical specifications.
3.0 REFERENCES
USP/BP
4.0 DEFINITIONS
Follow SOP Pharmaegg.com
5.0 SPECIFICATIONS USP/BP
TESTS SPECIFICATIONS
PHYSICAL ANALYSIS
1 Physical Form Crystalline Powder
2 Colour White to almost while
3 Test of Clarity & Colour Clear and colourless.
4 Solubility Sparingly soluble in water, freely soluble in chloroform.
5 Melting Point About 125°C with decomposition
6 pH 5.2 to 6.5 at 20°C to 25°C
7 Moisture Contents 3.5 to 5.5%
8 Water Contents(by Karl Fischer) Between 4 to 5.5%.
CHEMICAL ANALYSIS
9 Identification of Dextromethorphan Hydrobromide Raw Material Testing
10 Identification Test of Dextromethorphen Hydrobromide Greenish yellow colour should produce
11 Identification Test of Bromide Yellowish white precipitate should produce
12 Contents of Dextromethorphen Hydrobromide 99 to 101% OAB
6.0 SAMPLING
Refer to the determination Incoming SOPs for sampling.
7.0 REJECTIONS:
If the Dextromethorphan Hydrobromide does not satisfy the specifications mentioned in 5.0 then it will be rejected. In addition to the specifications, Dextromethorphan Hydrobromide is also rejected due to the following reasons:
7.1 If the receiving raw material is cross contaminated due to any reason.
7.2 The material does not bear 75% of its stated shelf life at the time of receipt.
8.0 PACKAGING
Dextromethorphan Hydrobromide is received in polyethylene bag placed in sturdy, cardboard container to protect it from moisture and light.
9.0 STORAGE: BP
Store in a well-closed container protected from light.
10.0 HANDLING
10.1 Use gloves & mask during weighing and dispensing operation of Dextromethorphan Hydrobromide.
10.2 Keep the container of Dextromethorphan Hydrobromide well closed immediately after use.
10.3 Place the container of Dextromethorphan Hydrobromide back to its specified area.
11.0 ANALYSIS
Suitable Machinery/Equipment/Apparatus
PHYSICAL CHEMICAL
1. Moisture Balance Graduated Pipette 1 ml
2. PH Meter Titration Flask 250 ml
3. Test Tubes Burette 25 ml
4. Beaker Analytical Balance
5. Glass Rod Spatula
6. Beaker 100 ml
7. FTIR,mortar & pestle
11.1 (B) List Of Reagent/Chemical
Chemicals
1. Ethanol 10 ml
2. Potassium bromide IR grade 200 mg
3. Chloroform 10 ml
Reagents
4. Silver Nitrate TS 5 ml 5. 1% w/v solution of ammonium molybdate in sulphuric acid 3 ml
11.2 PHYSICAL ANALYSIS USP/BP
11.2.1 Test of Physical Form:
Check the sample and confirm its physical form; it should be crystalline powder.
11.2.2 Test of Colour:
Confirm the colour of the material by comparing with standard from colour chart; it should be white to almost white.
11.2.3 Test of Clarity & Colour:
Dissolve 5 g of the sample in 100 ml of distilled water; the solution should be clear and colourless.
11.2.4 Test of pH
Weigh accurately on analytical balance 5 g of sample and make the volume upto 100 ml with distilled water. Take 50 ml from the resulting solution and measure the pH of solution at 30°C on pH meter; it should be 5.2 to 6.5 at 20°C to 25°C.
11.2.5 Test of Test of Solubility:
Check the solubility of the sample in Water and Chloroform.
It should be freely soluble in Chloroform and sparring soluble in water
11.2.6 Test of Loss on Drying:
Weigh accurately 10 g of sample on moisture balance. Adjust the temperature at 105°C, start drying the sample. At the end balance show percentage loss of moisture; moisture contents should be between 3.5 to 5.5%.
11.2.7 Water Contents:
Weigh accurately 50mg of sample and titrate for Karl Fischer water determination it should be between 4 to 5.5%.
11.2.8 Melting Point:
Check the melting point of sample; it should be about 125°C with decomposition.
11.3 Record the result of Physical Analysis on quality report.
11.4 CHEMICAL ANALYSIS: USP/BP
11.4.1 Examination of Dextromethorphan Hydrobromide by IR spectrum:
Take dried sample to 5mg of Dextromethorphan Hydrobromide and thoroughly mix with 95mg of dried standard of potassium bromide in pastel mortar.
Fill Macro cups with provided funnel like instrument and draw the spectrum it should comply with the standard spectrum.
11.4.2 Identification Test of Dextromethorphan Hydrobromide:
Weigh accurately on analytical balance 50 mg of the powdered sample, put it in the test tube, and add 2 ml of 1% w/v solution of ammonium molybdate in sulphuric acid; greenish yellow colour should produce.
11.4.3 Identification Test of Bromide
Weigh accurately on analytical balance 50 mg of the sample, put it in test tube, add 5 ml of distilled water, 1 ml of Silver Nitrate TS; yellowish white precipitate should produce.
11.4.4 Contents of Dextromethorphan Hydrobromide:
11.4.4.1 Sample Preparation:
11.4.4.1.1 Weigh accurately on analytical balance 100 mg of the powdered sample of Dextromethorphan Hydrobromide and make the volume upto 100 ml with distilled water in the volumetric flask.
11.4.4.1.2 Take 10 ml from the step 11.4.4.1.1 and make the volume upto 100 ml with distilled water in the volumetric flask and filter it.
11.4.4.1.3 Measure the absorption of step 11.4.4.1.2 at 278 nm on U.V Spectrophotometer.
11.4.4.1.4 Value of E ( 10%,1cm ) is 550.
11.4.4.2 Blank Preparation:
11.4.4.2.1Take 40 ml of distilled water and filter it. Dextromethorphan Hydrobromide Raw Material Testing.
11.4.4.2.2Measure the absorption of step 11.4.4.2.1 at 278 nm on U.V Spectrophotometer.
11.4.4.2.3Value of E ( 10%,1cm ) is 550.
Observation:
a) Absorption of Sample Preparation = A
b) Record the reading.
11.4.4.4. Calculations:
11.4.4.4.1 Calculate the contents of Dextromethorphan Hydrobromide as follows:
A
——————— x 100 = B
550
Limit: The contents of dextromethorphan hydrobromide should be between 99-101%. OAB
11.5 Record the result of Chemical Analysis on quality report.
Note. Incase of any non- conformance observed during Inspection and testing , Please Follow Quality System Procedure for Control of Non-Conforming Product.
12.0 RESPONSIBILITIES AND AUTHORITIES
1 Product Development Manager
2 Product Development Officer
3 Quality Control Manager
4 Quality Assurance Officer
5 Quality Assurance Assistant
6 Quality Assurance Attendant
COMPANY QUALITY FORMS:
1 Quality Report