Testing Procedure Cefotaxime Sodium
1.0 PURPOSE
This raw material specification and analysis prescribes the requirements for Cefotaxime Sodium (Sterile) which is used in Injection.
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/USP
4.0 DEFINITIONS
Follow Sop
5.0 SPECIFICATIONS USP/BP/USP
PHYSICAL ANALYSIS
1 Physical Form Fine Powder
2 Colour Off White
3 Reconstitution Time Not more than 1 minute
5 pH After Reconstitution 4.5 to 6.5 at 25°C +- 2°
6 Moisture Contents Not more than 5%
7 Reconstitution 2.1 ml +- 0.1 ml
8 Clarity Clear without any visible contamination
CHEMICAL ANALYSIS
9 Identification of Cefotaxime Sodium examination by IR spectrum Should comply the standard spectrum
10 Identification Test of Sodium Golden yellow colour flam should produce
11 Contents of Cefotaxime 85.5 to 100.2% On anhydrous basis
MICROBIOLOGICAL ANALYSIS
12 Potency Cefotaxime 85.5 to 100.2%
6.0 SAMPLING
Refer to the Incoming SOPs for sampling.
7.0 REJECTIONS:
If the Cefotaxime Sodium (Sterile) does not satisfy the specifications mentioned in 5.0 then it will be rejected. In addition to the specifications, Cefotaxime Sodium (Sterile) 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
Cefotaxime Sodium (Sterile) is received in polyethylene bag placed study, metallic container to protect it from moisture and light.
9.0 STORAGE: USP
Store in containers for sterile solids.
10.0 HANDLING
10.1 Use gloves & mask during weighing and dispensing operation of Cefotaxime Sodium (Sterile) in the sterile area.
10.2 Keep the container of Cefotaxime Sodium (Sterile) well closed immediately after use.
10.3 Place the container of Cefotaxime Sodium (Sterile) back to its specified area.
11.0 ANALYSIS
PHYSICAL
- Moisture Balance
- pH Meter
- Test Tubes
- Beaker
- Glass Rod
- Analytical Balance
- Test tubes
- Volumetric Flask 100 ml
- Graduated Pipette 1 ml
- Titration Flask 100 ml
- U.V. Spectrophotometer
- Analytical Balance
- Magnetic Stirrer
- Funnel
- Filter Paper Whatman No. 41
- Spatula
- Platinum Wire
- FTIR, mortar & pestle
Chemical
- Conc. HCl 2 ml
- Potassium bromide IR grade 200 mg
11.2 PHYSICAL ANALYSIS
11.2.1 Test of Physical Form:
Check the sample and confirm its physical form, it should be fine powder.
11.2.2 Test of Colour:
Confirm the colour of the material by comparing with standard from colour chart, it should be off white.
11.2.3 Test of Reconstitution:
Weigh accurately on analytical balance 263 mg of sample, put it in the vial, reconstitute it with 2 ml of Water for Injection, after reconstitution it should be 2.1 ml (± 0.1 ml).
11.2.4 Test of Clarity:
Weigh accurately on analytical balance 263 mg of sample, put it in the vial, reconstitute it with 2 ml of Water for Injection. After reconstitution check the clarity, it should be clear solution and without any visible contamination.
11.2.5 Test of Reconstitution Time:
Weigh accurately on analytical balance 263 mg of sample, put it in the vial, reconstitute it with 2 ml of Water for Injection and note the time, it should not be more than 1 minute.
11.2.6 Test of pH After Reconstitution:
Weigh accurately on analytical balance 100 mg of sample and make the volume upto 100 ml with distilled water in the beaker. Take 50 ml from the resulting solution and measure the pH of solution on pH meter; it should be 4.5 to 6.5 at 25°C +- 2°.
11.2.7 Test of Moisture Contents:
Weigh accurately 10 g of sample on moisture balance. Adjust the temperature at 85°C, start drying the sample. At the end balance show percentage loss of moisture, moisture contents should not be more than 5%.
11.3 Record the result of Physical Analysis on quality report.
11.4 CHEMICAL ANALYSIS: BP/USP
11.4.1 Examination of Cefotaxime by IR spectrum:
Take dried sample to 5mg of Cefotaxime sodium 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 be complies the standard spectrum.
11.4.2 Identification Test of Sodium:
Make the paste of 500 mg of the sample with 0.5 ml of concentrated hydrochloric acid, Moisten the platinum wire with the paste and introduce into the flame of a Bunsen Burner; golden yellow colour flame should produce.
11.4.3 Contents of Cefotaxime Sodium:
11.4.3.1 Standard Preparation:
11.4.3.1.1 Weigh accurately on analytical balance standard Cefotaxime Sodium equivalent to 100 mg of Cefotaxime Sodium, make the volume upto 100 ml with distilled water in the volumetric flask.
11.4.3.1.2 Take 1 ml from the step 11.4.3.1.1 and make the volume upto 100 ml with distilled water in the volumetric flask and filter it.
11.4.3.1.3 Measure the absorption of step 11.4.3.1.2 at 254 nm on U.V Spectrophotometer.
11.4.3.2 Sample Preparation:
11.4.3.2.1 Weigh accurately on analytical balance 100 mg of the powdered sample of Cefotaxime Sodium, make the volume upto 100 ml with distilled water in the volumetric flask.
11.4.3.2.2 Take 1 ml from the step 11.4.3.2.1 and make the volume upto 100 ml with distilled water in the volumetric flask and filter it.
11.4.3.2.3 Measure the absorption of step 11.4.3.2.2 at 254 nm on U.V Spectrophotometer.
11.4.3.3 Blank Preparation:
11.4.3.3.1 Take 40 ml of distilled water and filter it.
11.4.3.3.2 Measure the absorption of step 11.4.3.3.1 at 254 nm on U.V Spectrophotometer.
11.4.3.4 Observations:
a) Absorption of Sample Preparation = A
b) Absorption of Standard Preparation = B
c) Record the reading.
Calculations:
11.4.3.5.1 Calculate the contents of Cefotaxime Sodium as follows:
A
——————— x 100 = C
B
11.4.3.5.2 Limit: The contents of Cefotaxime should be between 85.5-100.2%. OAB.
11.5 Record the result of Chemical Analysis on quality report.
11.6 MICROBIOLOGICAL ANALYSIS
Follow SOPs .
Note. Incase of any non- conformance observed during Inspection and testing , Please Follow Quality System Procedure for Control of Non-Conforming Product.