SN/QC/SAPP/011

Department Quality Control Issue # 0 2

Section Quality Control Issue Date 0 3 - 2 0 1 5
THIS DOCUMENT IS NOT VALID WITHOUT SIGNATURES
STANDARD ANALYTICAL PROCEDURE PRODUCTS

PROCEDURE FOR ANALYSIS OF

TEROX 500 MG CAPSULES
(CIPROFLOXACIN 500 MG)(USP SPECS)
DRN………063466

WRITTEN BY SHMIM ARA QUALITY CONTROL ANALYST

REVIEWED BY SIRAJ AHMAD QUALITY CONTROL MANAGER
APPROVED BY AMIR IQBAL DIRECTOR OPERATION
This document is Property of SHAWAN Pharmaceuticals Page 1 of 8
 CONTENTS

AMMENDMENT 03

1.0 PURPOSE 04

2.0 SCOPE 04

3.0 PROCEDURE 04

4.0 RESPONSIBILITY …………………………………………………. 04

5.0 PRODUCT SPECIFICATIONS ……………………………………. 04

6.0 TESTS …………………………………………………………….. 05

6.1 INSTRUMENTS ……………………………………………………….05

6.2 REAGENTS ……………………………………………………………05

6.3 CHEMICAL ANALYSIS ……….05

6.3.1 IDENTIFICATION…………………………………….......................05

6.3.2 ASSAY (AFTER FINAL MIXING)…………..……………………..05

6.3.3 ASSAY FOR CAPSULES ………………………………………….. 05

6.3.4 HPLC METHOD (USP)………………………………………………. 06
6.3.5 Dissolution ……………………………………………………………..07
7.0 DOCUMENTATION ………………………………………………. 07
8.0 DISTRIBUTION …………………………………………………………07
 AMENDMENT SHEET

REV. # DATE INITIATED BY PAGE # NATURE OF AMENDMENT DONE BY

1.0 PURPOSE

This document is established to define the method of analysis for in process and finished product terox
500mg capsules to confirm its physical and chemical properties.

2.0 SCOPE

This procedure is applicable in the Quality Control Department for the analysis of Incoming product terox
500mg.

3.0 PROCEDURE
Collect the sample according to sampling procedure (sop number SN/QC/SOP/021) and analyze it
according to the standard analytical procedure.

4.0 RESPONSIBILITY:

ANALYST

MANAGER Q.C

5.0 PRODUCT SPECIFICATIONS

 Sr. # PARTICULARS AFTER MIXING AFTER filling AFTER COATING/
FINISHED

1. Physical Off white to white B/B color A blue color capsule.

Appearance granules. Capsule.
Identification Must be positive Must be positive Must be positive
for Ciprofloxacin for Ciprofloxacin for Ciprofloxacin

4. Disintegration NA N.M.T 15 min N.M.T.30min.

Time

5. Dissolution NA N.L.T 80.0% N.L.T 80.0%

6. Average weight Content wt=619mg 719mg ±2% 719mg ±2%

Shell wt=100mg
7. Assay Limit 90
–--------------------110%

6.0 TESTS

6.1 Instruments
a) Volumetric Flask 100 ml
b) Beakers
c) Test Tubes
d) Pipette 1, 2 ,10ml
e) Electric Balance
f) Hot air oven
g) Melting Point Apparatus
h) Spectrophotometer

6.2 Reagents/Chemicals
a) Distilled Water
b) Methanol
c) Hydrochloric acid solution.

6.3 Chemical Analysis

6.3.1 Identification:
Crush the capsules/ granules and make the solution of ciprofloxacin equivalent to 0.1 mg /ml.
Acidify 2ml of solution with 2M nitric acid; add 0.4ml of silver nitrate
Solution, shake and allow standing, a cruddy, white precipitate is produced.
Centrifuge and wash the precipitate with three 1ml quantities of water. Carry
Out this operation rapidly in subdued light, disregarding the fact that the
Supernatant solution may not become completely clear. Suspend the
Precipitate in 2ml of water and add 1.5ml of 10M ammonia, the precipitate

Dissolves easily with the possible exception of a few large particles

This dissolves slowly.

4.1 ASSAY (AFTER FINAL MIXING):

 SAMPLE PREPARATION:
Crush and transfer powder equivalent to 100mg of ciprofloxacin to a 100
ml volumetric flask, dilute with 0.1N HCl. Take 1 ml and dilute to 100 ml with same solvent. Measure the
absorbance at about 276 nm.

STANDARD PREPARATION:
Accurately weigh reference ciprofloxacin 100mg in 100 ml volumetric
flask and make up volume with 0.1N HCl. Take 1 ml and dilute to 100 ml with same solvent. Measure the
absorbance at about 276 nm.

OBSERVATION AND CALCULATIONS

%age = ABSORBANCE OF SAMPLE X 100

ABSORBANCE OF STANDARD

LIMIT: 90 ---------------- 110 %

6.3.3 ASSAY FOR CAPSULES:

SAMPLE PREPARATION:
Crush 10 capsules and transfer powder equivalent to 100mg of
ciprofloxacin to a 100 ml volumetric flask, dissolve and dilute with 0.1N HCl. Take 1 ml and dilute to 100
ml with same solvent. Measure the absorbance at about 276 nm.

STANDARD PREPARATION:
Accurately weigh reference equivalent to ciprofloxacin 100mg in 100
ml volumetric flask and make up volume with 0.1N HCl. Take 1 ml and dilute to 100 ml with same solvent.
Measure the absorbance at about 276 nm.

OBSERVATION AND CALCULATIONS

%age = ABSORBANCE OF SAMPLE X 100

ABSORBANCE OF STANDARD

LIMIT: 90 ---------------- 110 %

6.3.4 HPLC METHOD

Diluent— Prepare a filtered and degassed mixture of 0.025 M phosphoric acid, previously adjusted (with
triethylamine) to a pH of 2.0 ± 0.1, and acetonitrile (87:13).

Mobile phase— Prepare a filtered and degassed mixture of 0.025 M phosphoric acid, previously adjusted
with triethylamine) to a pH of 3.0 ± 0.1, and acetonitrile (87:13).

Standard preparation— Quantitatively dissolve an accurately weighed quantity of in Diluent to obtain a

solution having a known concentration of about 0.2 mg per mL.

Resolution solution— Dissolve a quantity of in the Standard preparation to obtain a solution containing
about 0.05 mg per mL.
Assay preparation— Transfer 5 capsules to a 500-mL volumetric flask, add about 400 mL of Diluent, and
sonicate for about 20 minutes. Dilute with Diluent to volume, and mix. Quantitatively dilute an accurately
measured volume of this solution, previously filtered through a 0.45-µm membrane filter, with Diluent to
obtain a solution containing the equivalent of about 0.20 mg of ciprofloxacin per mL.

Chromatographic system The liquid chromatograph is equipped with a 278-nm detector and a 4.6-mm ×

25-cm column that contains packing L1 and is operated at 30 ± 1 . The flow rate is about 1.5 mL per
minute.

Procedure— Separately inject equal volumes (about 10 µL) of the Standard preparation and the Assay
preparation into the chromatograph, record the chromatograms, and measure the peak areas for the
major peaks. Calculate the quantity, in mg, of ciprofloxacin (C17H18FN3O3) in each Tablet taken by the
formula:
(331.34/367.81)(CL/D)(rU / rS)

in which 331.34 and 367.81 are the molecular weights of ciprofloxacin and anhydrous ciprofloxacin
hydrochloride, respectively; C is the concentration, in mg per mL, of in the Standard preparation,
calculated on the anhydrous basis; L is the labeled quantity, in mg, of ciprofloxacin in each Tablet; D is
the concentration, in mg per mL, of ciprofloxacin in the Assay preparation, based on the labeled quantity
per Tablet and the extent of dilution; and rU and rS are the ciprofloxacin peak areas obtained from the
Assay preparation and the Standard preparation, respectively

Dissolution:
Medium: 0.01N HCl (900ml)
Apparatus: 50 rpm
Time: 30 minutes
Sample Preparation:
Take 6 Capsules and put 1 in each basket containing 0.01N HCl
medium. Start the apparatus at 50rpm for 30 min now take 25 ml of solution from each basket filter
it and then take 1.8 ml and dilute it to 100ml with 0.01N HCl. then scan it on 276nm against
standard

Standard Preparation
Weight 50mg of ciprofloxacin in 100ml flask make the volume with 0.01N HCl then take 1 ml and
dilute it in 50ml flask make the volume with the same solvent. Scan it on 276nm.

Calculation

%age Absorption of Sample x 100

Absorption of Standard

Tolerances— An amount of ciprofloxacin hydrochloride (C17H18FN3O3·HCl) equivalent to not less than

80% (Q) of the labeled amount of ciprofloxacin (C17H18FN3O3) is dissolved in 30 minutes.

7.0 DOCUMENTATION
Issue the certificate of analysis on its respective form and send the duplicate copy to production
department while retain the original copy in Q.C record.

8.0 DISTRIBUTION:

Master File.
Quality Control Manager.
Quality Control Analyst.