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Celecoxib Raw Material Testing

Celecoxib Raw Material Testing.

In this post, we share Celecoxib Raw Material Testing. You may also check our other Testing procedures here.

1.0 PURPOSE

This raw material specification and analysis prescribes the requirements for Celecoxib, which is one of the components of Capsule.

2.0 SCOPE

2.1 It is applicable in Materials, Product Development and Quality Assurance Department to confirm its physical and chemical specifications.

3.0 REFERENCES

Martindale / Manufacturer Specification

4.0 DEFINATIONS

Company Quality Manual

5.0 SPECIFICATIONS

Manufacturer Specification

PHYSICAL ANALYSIS

1 Physical Form Fine powder
2 Colour White to Off-White
3 Solubility Soluble in Methanol
4 Melting Point 158°C to 162°C
5 Loss on Drying Note more than 0.5 %

CHEMICAL ANALYSIS

6 Identification of Celecoxib examination by IR spectrum Should comply the standard spectrum
7 Identification of Celecoxib by Spectrophotometer The maximum absorption of 1% (1cm) of standard and sample preparation, should be at 252nm.
8 Content of Celecoxib 98.0 to 102.0 % (On Anhydrous basis)

6.0 SAMPLING

Refer to the Incoming SOPs for sampling.

7.0 REJECTIONS:

If the Celecoxib does not satisfy the specifications mentioned in 5.0 then it will be rejected. In addition to the specifications, Celecoxib 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 Celecoxib is received in thick aluminum foil bags placed in cardboard container to protect it from moisture and light.

9.0 STORAGE

Reference In house Specification.

9.1 Keep in a tightly closed container. Protect from physical damage. Store in a cool Below 25°C, dry, Ventilated area away from source of heat, ignition source.

10.0 HANDLING

10.1 Use gloves & mask during weighing and dispensing operation of Celecoxib.
10.2 Keep the container of Celecoxib well closed immediately after use.
10.3 Place the container of Celecoxib, 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

  • Bulb Pipette 1 ml
  • Volumetric Flasks 50ml ,100ml,1000ml
  • Sonicate Bath
  • Analytical Balance
  • Spatula
  • Beaker 100 ml
  • FTIR
  • HPLC
  • UV/Visible Spectrophotometer
  • Vacuum Pump
  • Ultrasonic Bath

Reagent

1. Potassium Dihydrogen Orthophosphate 2gm
2. Acetonitrile 550 ml
3. Methanol 10 ml
4. Potassium Bromide 100mg
5. 0.01M KH2PO4 450ml

11.2 PHYSICAL ANALYSIS

Manufacturer Specification

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 White to Off- white.

11.2.3 Test of Solubility:

Check the solubility of the sample in Methanol.
It should be Soluble in Methanol

11.2.4 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 not be more than 0.5%.

11.2.5 Test of Melting Point:

Take the powdered sample in the capillary tube meant for the purpose, put it in the Melting Point Apparatus. Check the temperature at which the powdered sample melts; melting point should be between 158°C-162°C.

11.2.6 Record the result of Physical Analysis on Quality report.

11.3 CHEMICAL ANALYSIS: Manufacturer Specification

11.4.1 Examination of Celecoxib by IR spectrum:

Take dried sample to 5mg of Celecoxib 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 Contents of Celecoxib By HPLC:

11.4.2.1 Chromatographic System

Instrument: A liquid Chromatograph equipped with UV- VIS detector
Column: Hichrom RPB C-18 X 4.6 mm , 5u or equivalent
Wave Length: 252 nm
Flow Rate: 1.0 ml/min
Injection Volume: 20ul

11.4.2.2. Mobile Phase

0.01M KH2PO4 and CH3CN in 45:55 ratio.

11.4.2.3.Preparation of 0.01M KH2PO4 SOLUTION

Take accurately about 0.68gm of Potassium Dihydrogen Orthophosphate and dissolve in 500ml water.

11.4.2.4 Preparation of Mobile Phase

Take 450ml of 0.01M KH2PO4 solution and add 550ml of Acetonitrile. Mix well. Filter by 0.45um Filter paper and degas.

11.4.2.5 Standard Preparation

Weigh accurately Equivalent to 50mg of the Working Standard and transfer into a 50ml volumetric flask. Dissolve in 20ml of Acetonitrile and make up the volume upto 50ml. With Acetonitrile. Take 10ml of this solution into 50ml volumetric flask and make up the volume Upto 50-ml with Acetonitrile.

11.4.2.6.Sample Preparation

Weigh accurately 50mg of the Sample and transfer into a 50ml volumetric flask. Dissolve in 20ml of Acetonitrile and make up the volume upto 50ml. With Acetonitrile. Take 10ml of this solution into 50ml volumetric flask and make up the volume upto50ml with Acetonitrile.

11.4.2.7. Procedure:

Equilibrate the Column for 30min with Mobile Phase. Inject exactly 20ul of blank solution (Acetonitril) in to the system and record the chromatogram.

Then Inject exactly 20ul of Standard preparation in to the system for Six times and record the Chromatograms.

The RSD of the principle peak area s of first five Injections of Standard preparation should not be more than 2.0%.

Inject exactly 20ul of test preparation in to the system and record the Chromatograms.

Calculate the Assay of the test sample using Sixth standard preparation area as Standard Area, Using the following Formula.

Area of Principle Peak of Sample x Weight of Standard taken x Purity % of Celecoxib WS x 100
Area of Principle Peak of Standard x Weight of Sample taken x ( 100 – LOD of test Sample)

11.4.2.8. Spectrophotometric analysis of Celecoxib

11.4.2.8.1 Identification

The maximum absorption of 1% (1cm) of standard and sample preparation should be at 252 nm.

11.4.2.8.2 Standard Preparation:

Dissolve equivalent to 100mg of celecoxib in methanol on ultrasonic bath and make up the volume with methanol = 100ml.

Take 1ml from the above solution and make up the volume to 100ml with Methanol, filter the solution before measure.

11.4.2.8.3 Sample Preparation:

Dissolve equivalent to 100mg of celecoxib on ultrasonic bath and make up the volume to 100ml with Methanol.
Take 1ml from above solution and make up the volume to 100ml with Methanol. Filter and measure the standard and sample preparation at 252nm taking methanol as blank.

11.4.2.8.4 Observation:

Absorption of sample X
Absorption of standard Y

11.4.2.8.5 Calculation:
                                                           X

Percentage contents of celecoxib ———————- x 100 = Z
                                                          Y
11.4.2.9 Limit: The contents of Celecoxib should be between 98 to 102% on anhydrous basis

11.4.2.10 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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