SN/QC/SAPP/002

Department Quality Control Issue # 0 3

Section Quality Control Issue Date 0 6 - 2 0 1 9
STANDARD ANALYTICAL PROCEDURE
CEFIXIME 400 MG CAPSULE

PROCEDURE FOR ANALYSIS OF

CEXIME 400 MG CAPSULES
(CEFIXIME 400 MG) (JP Specs)
DRN 049401

AMENDMENT

WRITTEN BY QC OFFICER

REVIEWED BY SENIOR QC OFFICER

APPROVED BY QC MANAGER

INITIATED
REV. # DATE PAGE # NATURE OF AMENDMENT DONE BY
BY
00 05.06.2007 USMAN ALL New Introduction

01 23.05.2013 SIRAJ ALL Updated as per Pharmacopeia

Formatting , Header and Footer, Page
02 03.03.2015 SIRAJ ALL
numbering
Formatting, Header and Footer, Addition
03 11.06.2019 HURRYAM ALL
of Technical section

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SN/QC/SAPP/002
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 6 - 2 0 1 9
STANDARD ANALYTICAL PROCEDURE
CEFIXIME 400 MG CAPSULE

CONTENTS

AMMENDMENT 01

1.0 PURPOSE 03

2.0 SCOPE 03

3.0 PROCEDURE 03

4.0 RESPONSIBILITY …………………………………………………. 03

5.0 PRODUCT SPECIFICATIONS …………………………………….. 03

6.0 TESTS …………………………………………………………….. 03

6.1 INSTRUMENTS ………………………….. 03

6.2 REAGENTS ………………………………. 03
4
6.3 CHEMICAL ANALYSIS……………………… 04

6.3.1 ASSAY (AFTER FINAL MIXING………………….. 04

6.3.2 ASSAY FOR CAPSULES ……………….…… 04
6.3.3 ASSAY BY HPLC…………………………. 05
6.3.4 DISSOLUTION………………………………… 05

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

8.0 REFRENCE …………………………………………………. 06

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 SN/QC/SAPP/002
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 6 - 2 0 1 9
STANDARD ANALYTICAL PROCEDURE
CEFIXIME 400 MG CAPSULE

1.0 PURPOSE
This document is established to define the method of analysis for in process and finished product Cexime
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 Cexime
capsules.

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 B/Blue COLOR B/Blue COLOR
Appearance powder FILLED CAPSULES. FILLED CAPSULES.
2 Identification Must be positive Must be positive Must be positive
For CEFIXIME for CEFIXIME for CEFIXIME
3. Disintegration - NMT 30min of the NMT 30min of the
Time(Shell) shell shell
4. CONTENT - 560mg/CAPSULE + 560mg/CAPSULE +
WT/CAPS 2% 2%
5. FILL WT/CAPS - 660mg/CAPS + 2% 660mg/CAPS + 3%
6. Assay Limit 90 –105%

6.0 TESTS

6.1 Instruments
a) Volumetric Flask 100 mL
b) Beakers
c) Pipette 1 mL
d) Electric Balance
e) Spectrophotometer.

6.2 Reagents/Chemicals

a) Distilled Water
b) Methanol
c) Octadecylsilanized silica gel
d) 0.05 M phosphoric acid
e) Monobasic potassium phosphate
f) Anhydrous dibasic sodium phosphate
g) Hydrochloric acid solution
h) Potassium phosphate
i) Acetonitrile

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 SN/QC/SAPP/002
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 6 - 2 0 1 9
STANDARD ANALYTICAL PROCEDURE
CEFIXIME 400 MG CAPSULE

6.3 Chemical Analysis

6.3.1 Identification:
Take few milligrams of powder containing Cefixime and dissolve in water add 2 mL of sulphuric acid
formaldehyde solution.shake and heat at spirit lamp for a while the solution will change its color to
yellowish green.

6.3.2 ASSAY (AFTER FINAL MIXING):

SAMPLE PREPARATION:
TEXT TECHNICAL
Weigh accurately 140mg powder equivalent to 100mg of 0.140gm 100mL buffer
cefixime to a 100 mL volumetric flask, dilute with buffer.
Take 1 mL and dilute to 100 mL with buffer. Measure the 1mL 100mL buffer
absorbance at about 288 nm. ʎ= 288nm

STANDARD PREPARATION:
TEXT TECHNICAL
Exactly weigh reference cefixime 112mg in 100 mL 0.12gm 100mL buffer
volumetric flask, dilute with buffer. Take 1 mL and dilute to
100 mL with buffer. Measure the absorbance at about 288 1mL 100mL buffer
nm. ʎ= 288nm

OBSERVATION AND CALCULATIONS

%age = ABSORBANCE OF SAMPLE X 100

ABSORBANCE OF STANDARD

LIMIT: 90 –105%
6.3.3 ASSAY FOR CAPSULES:
BUFFER PREPARATION:
Potassium dihydrogen phosphate 6.85g and sodium hydroxide pellets 0.92g in 1000mL water.

SAMPLE PREPARATION:
TEXT TECHNICAL
Empty 20 Capsules, Weigh accurately 140mg powder 0.140gm 100mL buffer
equivalent to 100mg of cefixime to a 100 mL volumetric
flask, dilute with buffer. Take 1 mL and dilute to 100 mL 1mL 100mL buffer
with buffer. Measure the absorbance at about 288 nm. ʎ=288nm

STANDARD PREPARATION:
TEXT TECHNICAL
Exactly weigh reference cefixime 112mg in 100 mL 0.12gm 100mL buffer
volumetric flask, dilute with buffer. Take 1 mL and dilute to
100 mL with buffer. Measure the absorbance at about 288 1mL 100mL buffer
nm. ʎ=288nm

OBSERVATION AND CALCULATIONS

%age = ABSORBANCE OF SAMPLE X 100

ABSORBANCE OF STANDARD

LIMIT: 90 –105%

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SN/QC/SAPP/002
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 6 - 2 0 1 9
STANDARD ANALYTICAL PROCEDURE
CEFIXIME 400 MG CAPSULE
6.3.4 (HPLC METHOD)

Sample preparation:
TEXT TECHNICAL
Take out the contents of NLT 20 cefixime capsules, weigh 0.1 g 100mL (0.1mol/L phosphate)
accurately the mass of the contents and powder. Weigh
accurately a portion of powder, equivalent to about 0.1g of 10mL 50mL (0.1mol/L phosphate)
Cefixime hydrate add 70mL of 0.1 mol/L phosphate buffer
solution (pH 7.0) and shake for 30 min, add 0.1 mol/L
phosphate. Buffer solution to make exactly 100mL.
Centrifuge this solution, pipette 10 mL of supernatant
liquid, add 0.1mol/L phosphate buffer solution to make
exactly 50mL and use this solution as Sample solution.

Standard solution:
TEXT TECHNICAL
Separately, weigh accurately an amount of cefixime RS 20mg 100mL (0.1mol/L phosphate)
equivalent to about 20mg dissolve in 0.1 mol/L Phosphate
buffer solution to make exactly 100mL, and use this
solution as standard solution.

Amount[mg(potency)] of Cefixime = Ms* At/As*5

Operating Conditions:
Detector: UV 254
Column: a Stainless Steel column 4mm in inside diameter and 125mm in length packed with Octadecylsilanized
silica gel for LC.
Column temperature: 40oC
Flow Rate: Adjust so that the retention time of cefixime is about 10 minutes.

6.3.5 DISSOLUTION:

Medium: 0.05M phosphate Buffer, 900mL

0.05M Buffer: 2.75 mL phosphoric acid in 1000mL
Apparatus: 1: 100 rpm.
Time: 10, 20, 30, 45, 60 minutes.
Limit: NLT 80 %(Q)
Instrumental conditions:
Mode: UV
Analytical wavelength: 228nm

Standard solution:
TEXT TECHNICAL
Dissolve 0.0559g of Cexime in 50 mL of phosphate buffer, 0.0559 g 50mL
and dilute 1mL in phosphate buffer and make up volume 1mL 50mL
upto 50mL. ʎ = 228 nm

Sample solution:
TEXT TECHNICAL
Add one capsule in each basket, volume of 900mL 0.05M 1 capsule 900mL phosphate buffer
phosphate buffer, dissolve 400mg of Cexime (one capsule) 5mL 100 mL
in 900 mL of phosphate buffer, and take sample of 5mL Filter (0.45µm)
and make up volume upto 100mL. Filter through 0.45-µm ʎ= 228nm
filter.

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SN/QC/SAPP/002
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 6 - 2 0 1 9
STANDARD ANALYTICAL PROCEDURE
CEFIXIME 400 MG CAPSULE
7.0 DOCUMENTATION:

 Request for Analysis

 Certificate of Analysis
 Inprocess Register
 Instrument Log Books
 Batch Manufacturing Record

8.0 REFRENCE:

 JP XVII: Page 625

 Dissolution: FDA.