Ceftriaxone Sodium Sterile Raw Material Testing
1.0 PURPOSE
This raw material specification and analysis prescribes the requirements for Ceftriaxone Sodium Sterile, which is one of the components of Injection.
2.0 SCOPE
2.1 It is applicable in materials, Product Development and Quality Assurance Department to confirm its Physical and Chemical specifications.
2.2 Item Code No…..
3.0 REFERENCES
BP/USP/Martindale 31st Edition /Merck Index 12th Edition/ In-house
4.0 DEFINITIONS
Company Quality Manual
5.0 SPECIFICATIONS
Reference Martindale 31st Edition /USP/ Merck Index/ In-house Specifications.
TESTS AND SPECIFICATIONS
PHYSICAL ANALYSIS
1. Physical: Form Crystalline Powder
2. Colour: Almost white to yellowish
3. Color after reconstitution: Light yellow
4. Reconstitution Time: Not more than 3 minute
5. pH: After Reconstitution 6.0 to 8.0 at 30°C
6. Moisture Contents: Not more than 11.0% at 105°C
7. Water Contents(by Karl Fischer): Between 8 to 11%.
8. Reconstitution: 2.1 ml (±0.1 ml)
9. Clarity: Clear Solution without any visible contamination
10. Bulk Density: 0.200 – 0.400 g/ml
11. Tapped Density: 0.400 – 0.600 g/ml
CHEMICAL ANALYSIS
1. Examination of Ceftriaxone Sodium Sterile by IR spectrum Should comply with the standard spectrum
2. Identification of Ceftriaxone Sodium Sterile Greenish-yellow color should produce which becomes yellow after heating on water bath
3. Identification of Sodium Golden yellow colour flame should produce
4. Content of Ceftriaxone Not Less Than 79.5% ( On anhydrous basis)
MICROBIOLOGICAL ANALYSIS
1. Potency of Ceftriaxone Sodium Sterile 96-102%
6.0 SAMPLING
Refer to the Incoming SOPs for sampling.
7.0 REJECTIONS:
If the Ceftriaxone Sodium Sterile does not satisfy the specifications mentioned in 5.0 then it will be rejected. In addition to the specifications, Ceftriaxone 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
8.1 Ceftriaxone Sodium Sterile is received in thick aluminum foil bags placed in containers for solid sterile solids.
9.0 STORAGE Reference BP
9.1 The sealed container should be stored at a temperature not exceeding 30°C.
10.0 HANDLING
10.1 Use gloves & mask during weighing and dispensing operation of Ceftriaxone Sodium Sterile.
10.2 Keep the container of Ceftriaxone Sodium Sterile well closed immediately after use.
10.3 Place the container of Ceftriaxone Sodium Sterile, back to its specified area.
11.0 ANALYSIS
11.1 (A) Suitable Machinery/Equipment/Apparatus
PHYSICAL
- Moisture Balance
- Analytical Balance
- Test Tubes
- Beaker
- Glass Rod
- CHEMICAL
- Graduated Pipette 1 ml
- Volumetric flasks100ml
- UV-Visible Spectrophotometer
- Analytical Balance
- Spatula
- Beaker 100 ml
- FTIR, Mortar, Pastel
Chemicals
1. Methanol 10ml
2. Ethanol 10ml
3. Concentrated Hydrochloric Acid 1.0ml
Reagents
1. Sulfuric Acid + Formaldehyde solution 2.0ml
11.2 PHYSICAL ANALYSIS Reference Martin Dale/BP/USP, In-house specifications.
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 color of the material by comparing it with standard from the colour chart; it should be almost white to yellowish.
11.2.3 Test of Reconstitution:
Weigh accurately on analytical balance 595 mg of sample on weighing balance, put it in the vial and add 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 595 mg of sample, put it in the vial, and 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 595 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 3 minute.
11.2.6 Colour after Reconstitution:
Weigh accurately on analytical balance 595 mg of sample on weighing balance, put it in the vial, reconstitute it with 2 ml of Water for Injection; after reconstitution colour should be light yellow.
11.2.7 Test of pH After Reconstitution:
Check the pH of reconstituted sample (step11.2.3); it should be 6.0 to 8.0 at 30°C.
11.2.8 Test of Moisture Contents:
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 not be more than 11.0%.
11.2.9 Water Contents:
Weigh accurately 50mg of sample and titrate for Karl Fischer water determination it should be between 8 to 11%.
11.2.10 Bulk Density:
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 0.200 – 0.400 g/ml.
11.2.11 Tapped Density:
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 0.400 – 0.600 gm/ml.
11.2.11 Record the result of Physical Analysis on Quality report.
11.3 CHEMICAL ANALYSIS:
BP/ Merck Index/ USP.
11.3.1Examination of Ceftriaxone Sodium Sterile by IR spectrum:
Take dried sample equivalent to 5mg of Ceftriaxone Sodium Sterile 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 comply with the standard spectrum.
11.3.2 Identification of Ceftriaxone Sodium Sterile:
Take about 10mg of sample in test tube, moisten with 0.05ml of water and add 2ml of Sulphuric Acid – Formaldehyde reagent. Mix the contents of the test tube by swirling; The solution is greenish-yellow. Place the test-tube in a water- bath for 1min. a yellow colour should develop.
11.3.3 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.
11.3.4. Contents of Ceftriaxone :
11.3.4.1Standard Preparation:
Weigh accurately on analytical balance standard equivalent to 100mg of Ceftriaxone, make the volume upto 100 ml with distilled water in the volumetric flask.
Take 1 ml from the above step and make the volume upto 100ml with distilled water in the volumetric flask and filter it. And Measure the absorption at 242nm on UV- Visible Spectrophotometer. 100mg of Ceftriaxone = 119.0 mg of Ceftriaxone Sodium
11.3.4.2 Sample Preparation:
Weigh accurately on analytical balance 100 mg of the powdered sample of Ceftriaxone Sodium Sterile, make the volume upto 100 ml with distilled water in the volumetric flask.
Take 1 ml from the above step and make the volume upto 100ml with distilled water in the volumetric flask and filter it. And Measure the absorption at 242nm on UV- Visible Spectrophotometer.
11.3.4.3 Blank Preparation:
Take 40 ml of distilled water and filter it. And Measure the absorption at 242nm on UV-Visible Spectrophotometer.
11.3.4.4 Observations:
a) Absorption of Sample Preparation = A
b) Absorption of Standard Preparation = B
c) Record the reading.
11.3.4.5 Calculations:
Calculate the contents of Ceftriaxone Sterile as follows:
A
——————— x 100 = C
B
Limit: The contents of Ceftriaxone should not be less than 79.5%. (On anhydrous basis)
11.3.4.6 Record the result of Chemical Analysis on Quality report.
Note: Incase of any non-conformance observed during inspection and testing please follow Procedure for Non-Conforming of Product.
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