In this post, we have explained how to perform testing Ciprofloxacin Hydrochloride Raw Material in pharmaceuticals.
1.0 PURPOSE
It is established to describe specification and analysis of Ciprofloxacin Hydrochloride, which is one of the components of Tablet.
2.0 SCOPE
It is applicable in Material, Product Development and Quality Assurance Department to confirm its physical and chemical specifications.
3.0 REFERENCES
USP/BP/inhouse
4.0 DEFINITION
Follow SOPs
5.0 SPECIFICATIONS USP/BP/inhouse
PHYSICAL ANALYSIS
- Physical Form Crystalline powder
- Colour Faintly Yellow to light yellow
- pH 3.0—4.5 at 25°C ± 2°.
- Melting point Should be between 318—320°C.
- Moisture Content Should be between 4.7—6.7 %.
- Water Contents (by karl Fischer) Between 4.7 to 6.7%
CHEMICAL ANALYSIS
Identification of Chloride White ppt. should produce
Identification of Ciprofloxacin Red ppt. Should produce.
Contents of Ciprofloxacin HCl Should be between 98-102 % on anhydrous basis.
6.0 SAMPLING
Refer to the Incoming SOPs for sampling .
7.0 REJECTIONS:
If the Ciprofloxacin Hydrochloride does not satisfy the specifications mentioned in 5.0 then it will be rejected. In addition to the specifications, Ciprofloxacin Hydrochloride 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
Ciprofloxacin Hydrochloride is received in plastic/ metallic container placed in sturdy, cardboard container to protect it from moisture and light.
9.0 STORAGE: USP
Store in tight, light resistant container.
10.0 HANDLING
Use gloves & mask during weighing and dispensing operation of Ciprofloxacin Hydrochloride and keep the container well closed immediately after use. Keep the container of Ciprofloxacin HCL back to its specified area.
10.0 ANALYSIS
11.1 (A) Suitable Machinery/Equipment/Apparatus
- Moisture Balance
- pH Meter
- Test Tubes
- Beaker
- Glass Rod
- Analytical Balance
- Melting Point Apparatus
- Test tubes
- Volumetric Flask, 100 ml,
- Graduated Pipette 1 ml, 10ml
- Titration Flask 100 ml
- UV Spectrophotometer.
- Analytical Balance
- Spatula
11.1 (B) List Of Reagent/Chemical
1- Silver Nitrate TS 2ml
2- Ferric Chloride TS 5ml
11.2 PHYSICAL ANALYSIS: USP/BP/inhouse
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; it should be Faintly Yellow to Light yellow.
11.2.3 Test of pH:
Weigh accurately equivalent to 1 gm of Ciprofloxacin HCl on sensitive weighing balance, dissolve it in 40 ml of water & measure the pH at 25 °C 2° on pH meter, it should be between 3.0 to 4.5.
11.2.4 Test of Melting point:
Check the melting point of Ciprofloxacin on melting point apparatus, it should be between 318—320°C.
11.2.5 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 shows percentage loss of moisture; moisture contents should be between 4.7—6.7%.
11.2.6 Water Contents:
Weigh accurately 50mg of sample and titrate for Karl Fischer water determination it should be between 4.7 to 6.7%.
11.3 Record the result of Physical Analysis on quality report.
11.4 CHEMICAL ANALYSIS: USP/BP/inhose
11.4.1 Identification Test of Chloride:
Weigh accurately on analytical balance 20 mg of the sample, put it in the test tube, add 10ml of distilled water, 1 ml of silver nitrate TS, white ppt. should produce.
11.4.2 Identification Test of Ciprofloxacin:
Weigh accurately on analytical balance 20 mg of the sample, put it in the test tube, add 10ml of distilled water, 1 ml of Ferric Chloride TS , Red colour Should produce.
11.4.3 Contents of Ciprofloxacin Hydrochloride.
11.4.3.1 Standard Preparation:
Weigh accurately on analytical balance reference standard Ciprofloxacin Hydrochloride equivalent to 50 mg of Ciprofloxacin Hydrochloride, add 50 ml of distilled water & make the volume up to 100 ml with distilled water. Take 1ml from the above solution and make the volume 100ml with distilled water. Filter & measure the absorption at 276 nm.
11.4.3.2 Sample Preparation:
Weigh accurately on analytical balance sample of Ciprofloxacin Hydrochloride equivalent to 50 mg of Ciprofloxacin Hydrochloride, add 50 ml of distilled water & make the volume up to 100 ml with distilled water. Take 1ml from the above solution and make the volume 100ml with distilled water. Filter & measure the absorption at 276 nm.
11.4.3.3 Blank Preparation:
Take 40 ml of distilled water. Filter & measure the absorption at 276 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.
11.4.3.5 Calculations:
Calculate the contents of Ciprofloxacin Hydrochloride as follows:
A
————— x 100 = C
B
Limit: The contents of Ciprofloxacin Hydrochloride should be between 98-102% on anhydrous basis.
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.