SN/QC/SAPP/012

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
WADIN 250 MG CAPSULE
(CEPHRADINE 250 MG/Cap)(USP Specs)
DRN ………….. 049403

WRITTEN BY SHAMIM ARA QUALITY CONTROL ANALYST

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

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 ASSAY (AFTER FINAL MIXING……………….. 05
6.3.2 ASSAY FOR FILLED CAPSULE…. …………… 05

6.3.3 DISSOLUTION ……………………………..……. 06

6.3.4 HPLC METHOD …………………….……………. 06

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 Cephradine
suspension 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 Cephradine
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

BLISTERING
1. PHYSICAL White to Off white powder BLUE/WHITE COLORED FILLED
APPEARANCE CAPSULES

2. IDENTIFICATION Must be positive Must be positive

for Cephradine for Cephradine

3. D.TIME NA NMT 15 min

4. CONTENT WT NA 334mg/cap
5. FILL WT /UNIT NA 414 Mg+ 3%
6. ASSAY LIMIT 90---------------- 120 %

7. LOD NMT 7% NMT 7%

8 DISSOLUTION NA NLT 75%

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) 0.1NHCL

6.3 Chemical Analysis

6.3.1 ASSAY (AFTER FINAL MIXING):

SAMPLE PREPARATION:
Weigh accurately sample powder equivalent to 100mg of Cephradine to a 100
ml volumetric flask, dilute with 0.1 N HCl, sonicate the flask and filter the solution Take 2ml filtrate and dilute to 50
ml with same solvent. Measure the absorbance at about 255 nm.

STANDARD PREPARATION:
Exactly weigh reference standard Cephradine 100mg in 100 ml volumetric
flask and make up volume with 0.1 HCl. sonicate the flask Take 2 ml and dilute to 50 ml with same solvent.
Measure the absorbance at about 255nm.

OBSERVATION AND CALCULATIONS

%Age = ABSORBANCE OF SAMPLE X 100

ABSORBANCE OF STANDARD

LIMIT: 90 –---------------120%

6.3.2 ASSAY FOR FILLED CAPSULE;

SAMPLE PREPARATION:
Weigh accurately 10 capsules and transfer powder equivalent to 100mg of
Cephradine to a 100 ml volumetric flask, dilute with 0.1 N HCl, filter and then Take 2ml and dilute to 50 ml with
same solvent. Measure the Absorbance at about 255 nm.
.

STANDARD PREPARATION:
Accurately weigh reference standard equivalent to Cephradine 100mg in
100 ml volumetric flask and make up volume with 0.1 N HCl. Take 2 ml and dilute to 50 ml with same solvent.
Measure the Absorbance at about 255 nm.

OBSERVATION AND CALCULATIONS

%Age = ABSORBANCE OF SAMPLE X 100

ABSORBANCE OF STANDARD

LIMIT: 90 –---------------120%

6.3.3 DISSOLUTION
Medium 0.12N Hcl

Apparatus 100 RPM

Time 45min

Procedure determine the amount of cephradine dissolved from UV absorbance at the wavelength of maximum
absorbance at about 255nm a filtered portion of solution under test, suitably diluted with dissolution medium, if
necessary in comparison with a standard solution having a known concentration of USP cephradine in the same
media.
Tolerance not less than 75% of the labeled amount of cephradine is dissolved in 45 minutes.

6.3.4 HPLC METHOD (USP)

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). Make adjustments if necessary (see System
Suitability under

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 Tablets 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.
Chromatograph the Resolution solution, and record the peak responses as directed for Procedure: the retention
time for ciprofloxacin is between 6.4 and 10.8 minutes; the relative retention times are about 0.7 for ciprofloxacin
ethylenediamine analog and 1.0 for ciprofloxacin; and the resolution, R, between the ciprofloxacin
ethylenediamine analog peak and the ciprofloxacin peak is not less than 6. Chromatograph the Standard
preparation, and record the peak responses as directed for Procedure: the column efficiency, determined from
the ciprofloxacin peak, is not less than 2500 theoretical plates; the tailing factor for the ciprofloxacin peak is not
more than 2.0; and the relative standard deviation for replicate injections is not more than 1.5%.

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.

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.