SN/QC/SAPP/013

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 500 MG CAPSULE
(CEPHRADINE 500 MG/Cap)(USP Specs)
DRN ………….. 049404

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

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 ASSAY (AFTER FINAL MIXING……………….. 05

6.3.2 ASSAY FOR filled Capsule ………… ………… 05

6.3.3 DISSOLUTION …………………………………… 05
6.3.4 Assay by HPLC …………………………..……… 05

7.0 DOCUMENTATION ………………………………….……….06

8.0 DISTRIBUTION ……………………………………….……… 06
 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 wadin capsule
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 Wadin.
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 Off white to yellow color BLUE/ BLUE COLORED FILLED
APPEARANCE powder CAPSULES
2. IDENTIFICATION Must be positive Must be positive
for cephradine for cephradine
3 CONTENT WT NA 500mg/cap

4 FILL WT /UNIT NA 660mg+ 3%

5 ASSAY LIMIT 90---------------------- 120%

6 D.T NA NMT 15MINTUES

7 LOD NMT 7% NMT 7%

08 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) Titration Flask
f) Electric Balance
g) Hot air oven
h) Melting Point Apparatus
i) Spectrophotometer

6.2 Reagents/Chemicals
a) Distilled Water
b) Hydrochloric acid solution.
6.3 Chemical Analysis

6.3.1 ASSAY (AFTER FINAL MIXING):

SAMPLE PREPARATION:
Weigh accurately and transfer powder equivalent to 100mg of cephradine to a 100 ml volumetric flask,
dilute with 0.1 N HCl. Take 2ml and dilute to 50 ml with same solvent. Measure the absorbance at about
288 nm.
STANDARD PREPARATION:
Accurately weigh reference cephradine 100mg in 100 ml volumetric flask and make up volume with
0.1 Hcl. Take 2 ml and dilute to 50 ml with same solvent. Measure the absorbance at about 288nm.
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 and transfer powder equivalent to 100mg of cephradine to a 100 ml volumetric flask,
dilute with 0.1 N HCl. Take 2ml and dilute to 100 ml with same solvent. Measure the absorbance at about
255 nm.
.

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

OBSERVATION AND CALCULATION

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 Assay by HPLC (USP)

Mobile phase, Standard preparation, Resolution solution, and Chromatographic system— Proceed as
directed in the Assay under Cephradine.

Assay preparation— Transfer, as completely as possible, the contents of not fewer than 20 Capsules to a
suitable tared container, determine the average weight per Capsule, and mix the combined contents.
Transfer an accurately weighed portion of the powder, equivalent to about 125 mg of cephradine, to a
250-mL volumetric flask, add 50 mL of Mobile phase, sonicate for about 15 minutes, and shake by
mechanical means for about 10 minutes. Dilute with Mobile phase to volume, and mix. Filter a portion of
 this mixture through a filter having a porosity of 0.5 µm or finer, discarding the first 5 mL of the filtrate.
Use the filtrate as the Assay preparation.

Procedure— Separately inject equal volumes (about 10 µL) of the Standard cephradine preparation and
the Assay preparation into the chromatograph, record the chromatograms, and measure the responses
for the major peaks. Calculate the quantity, in mg, of cephradine (sum of cephradine and cephalexin) in
the portion of Capsules taken by the formula:
0.25CP(rU / rS)

in which C is the concentration, in mg per mL, of in the Standard preparation; P is the designated
potency, in µg per mg, of and rU and rS are the sums of the cephradine and cephalexin peak responses
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.