How To Test Cloxacillin Sodium Raw Material PURPOSE
This raw material specification & analysis prescribes the requirements for How To Test Cloxacillin Sodium Raw Material which is used in Capsules.
This raw material specification & analysis prescribes the requirements for Cloxacillin Sodium (Compacted) which is one of the component of Capsule.
It is applicable in Material Department, Product Development and Quality Assurance Department to confirm its physical and chemical specifications.
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1. Physical Form Granular Powder
2. Colour White to almost white
3. Clarity & Colour Clear & Colourless
4. Solubility Freely soluble in water, methanol &, soluble in ethanol.
5. pH 5.0 to 7.0 at 25°C +-2°
6. Moisture Contents Not more than 5%
7. Water Contents(by Karr Fischer) Between 3 to 4.5%.
8. Bulk Density 0.400 – 0.600 g/ml
9. Tapped Density 0.450 – 0.800 g/ml
10. Identification of Cloxacillin examination by IR spectrum Should comply the standard spectrum
11. Identification Test of Cloxacillin Slightly greenish yellow colour should produce
12. Identification Test of Sodium Golden yellow coloured flame should produce
13. Content of Cloxacillin Sodium 95 to 101%
14. Potency of Cloxacillin Sodium 95 to 101%
Refer to the Incoming SOPs for sampling and determination (Follow SOP pharmaegg.com)
If the Cloxacillin Sodium (Compacted) does not satisfy the specifications mentioned in 5.0 then it will be rejected. In addition to the specifications, Cloxacillin Sodium (Compacted) is also rejected due to the following reasons:
1 If the receiving raw material is cross contaminated due to any reason.
2 The material does not bear 75% of its stated shelf life at the time of receipt.
Cloxacillin Sodium (Compacted) is received in polyethylene bag placed studry, cardboard container to protect it from moisture and light.
Store the sealed container at a temperature not exceeding 25°C.
1 Use gloves & mask during weighing and dispensing operation of Cloxacillin Sodium (Compacted).
2 Keep the container of Cloxacillin Sodium (Compacted) well closed immediately after use.
3 Place the container of Cloxacillin Sodium (Compacted) back to its specified area.
1. Moisture Balance Test tubes
2. PH Meter Volumetric Flask 500ml,100 ml, 50 ml
3. Test Tubes Graduated Pipette 2 ml
4. Beaker Titration Flask 100 ml
5. Glass Rod U.V. Spectrophotometer
6. Analytical Balance
7. – Magnetic Stirrer
8. – Funnel
9. – Filter Paper Whatman No. 41
10. – Beaker 100 ml
11. – Spatula
12. – FTIR, mortar & pestle
1. Ethanol (96%) 10 ml
2. Methanol 110 ml
3. Conc. Sulphuric Acid 1 ml
4. Potassium bromide IR grade 200 mg
5. Conc. Hydrochloric Acid 1 ml
6. 0.1 N Sulphuric Acid 300 ml
PHYSICAL ANALYSIS USP/BP/Inhouse
Test of Physical Form:
Check the sample and confirm its physical form; it should be granular powder.
Test of Colour:
Confirm the colour of the material by comparing with standard from colour chart; it should be white to almost while. How To Test Cloxacillin Sodium
Test of Clarity & Colour:
Weigh accurately on analytical balance 100 mg of sample, put it in the test tube, and dissolve it in 10 ml of distilled water; it should be clear and colourless. How to Test Cloxacillin Sodium
Test of pH:
Weigh accurately on analytical balance 10 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 25°C2° on pH meter; it should be 5.0 to 7.0 at 25°C 2°.
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%.
Weigh accurately 50mg of sample and titrate for Karl Fischer water determination it should be between 3 to 4.5%.
Test of Solubility:
Check the solubility of the sample in water, methanol and ethanol.
It should be freely soluble in water, methanol and soluble in Ethanol.
Take sample in the measuring cylinder, the surface level of the sample in the cylinder should be even, note the volume without tapping, it should be between 0.400 – 0.600 g/ml.
Take sample in the measuring cylinder, the surface level of the sample in the cylinder should be even, note the volume with tapping, it should be between 0.450 – 0.800 gm/ml.
Record the result of Physical Analysis on quality report.
CHEMICAL ANALYSIS: USP/BP/Inhouse
Examination of Cloxacillin by IR spectrum:
Take dried sample to 5mg of Cloxacillin 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.
Identification Test of Cloxacillin:
Weigh accurately on analytical balance 20 mg of the sample, put it in the test tube, add 0.5 ml of distilled water, 0.5 ml of Conc. Sulphuric Acid; slightly greenish yellow colour appears.
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.
Contents of Cloxacillin Sodium
Weigh accurately on analytical balance reference standard Cloxacillin Sodium equivalent to 100 mg of Cloxacillin Sodium, add 10 ml of Methanol, mix it for 15 minutes, make the volume upto 50 ml with Methanol in volumetric flask and filter it in 100 ml titration flask.
Take 2 ml from the step 188.8.131.52.1 and make the volume upto 100 ml with 0.1 N Sulphuric Acid.
Sample Preparation :
- Titrate the compacted sample in a mortar with the help of pastle till it becomes fine powder.
- Weigh accurately on analytical balance 100 mg of powdered sample of Cloxacillin Sodium, add 10 ml of Methanol, mix it for 15 minutes, make
- the volume upto 50 ml with Methanol in volumetric flask and filter it in 100 ml titration flask.
- Take 2 ml from the step 184.108.40.206.2 and make the volume upto 100 ml with 0.1 N Sulphuric Acid.
- Measure the absorption at 344 nm on U.V Spectrophotometer after exactly 45 minutes.
Take 40 ml of 0.1 N Sulphuric Acid.
Measure the absorption of step 220.127.116.11.1 at 344 nm on U.V Spectrophotometer after exactly 45 minutes.
a) Absorption of Sample Preparation = A
b) Absorption of Standard Preparation = B
c) Record the reading.
18.104.22.168.1 Calculate the contents of Cloxacillin Sodium as follows:
—————– x 100 = C
Limit: The contents of Cloxacillin Sodium should be between 95-101%.
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 Follow SOP pharmaegg.com
MICROBIOLOGICAL ANALYSIS :
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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:
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