SN/QC/SAPP/015

Department Quality Control Issue # 0 3

Section Quality Control Issue Date 0 1 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE XEGTIN 20MG CAPSULES

PROCEDURE FOR ANALYSIS OF

XEGTIN 20MG CAPSULES
(PIROXICAM BETA CYCLODEXTRIN
BETA CYCLODEXTRIN 20MG)
(SHAWAN’S Specs)
DRN………………052672

AMENDMENT SHEET

REV. # DATE INITIATED BY PAGE # NATURE OF AMENDMENT DONE 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 14.1.20 HURRYAM ALL
of Technical section

WRITTEN BY QC OFFICER

REVIEWED BY SENIOR QC OFFICER

APPROVED BY QC MANAGER

1
SN/QC/SAPP/015
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 1 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE XEGTIN 20MG CAPSULES

CONTENTS

1.0 AMMENDMENT 01

2.0 PURPOSE 03

3.0 SCOPE 03

4.0 PROCEDURE 03

5.0 RESPONSIBILITY …………………………………………………. 03

6.0 PRODUCT SPECIFICATIONS …………………………………….. 03

7.0 TESTS …………………………………………………………….. 03

7.1 INSTRUMENTS ………………………………………. 03

7.2 REAGENTS ……………………………………………. 03

7.3 CHEMICAL ANALYSIS ………………………………. 04

7.3.1 IDENTIFICATION 04

7.3.2 ASSAY BY SPECTROPHOTOMETER………………… 04

7.3.3 DISSOLUTION …………………………………………….. 04

7.3.4 ASSAY AFTER FILLING……………………………….…. 05

8.0 DOCUMENTATION ……………………………………………….. 05

9.0 REFERENCE ……………………………………………..………. 05

2
 SN/QC/SAPP/015
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 1 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE XEGTIN 20MG CAPSULES
2.0 PURPOSE

This document is established to define the method of analysis for in process and finished product Xegtin capsule
to confirm its physical and chemical properties.

3.0 SCOPE

This procedure is applicable in the Quality Control Department for the analysis of Incoming product Xegtin
capsule.

4.0 PROCEDURE

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

5.0 RESPONSIBILITY:

ANALYST

MANAGER Q.C

6.0 PRODUCT SPECIFICATIONS

Sr. # PARTICULARS MIXED POWDER FILLED CAPSULES FINISHED

PRODUCT
1. Physical Light Yellow to white Light Yellow Color Powder filled in orange
Appearance color powder color capsules

2. Identification Must be positive

for Piroxicam Beta Cyclodextrin
3. Average weight - 330mg ± 2%

4. Disintegration - N.M.T 15 min N.M.T.15 min.

Time
7. Assay Limit 92.5 – 107.5%

8. Dissolution NLT 85%

9. Content uniformity As per uniformity of content formula

7.0 TESTS

7.1 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

7.2 Reagents/Chemicals
a) Distilled Water
b) Acetonitrile (ACN)
c) Methanol
3
SN/QC/SAPP/015
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 1 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE XEGTIN 20MG CAPSULES
d) HCl

7.3 Chemical Analysis

7.3.1 IDENTIFICATION:
Prepare 10 microgram per liter solution of Piroxicam Beta Cyclodextrin standard and sample by dissolving
them in methanolic HCl and record spectra from 200 to 400 nm both sample and standard solution give
absorption maxima at 358 nm.

7.3.2 ASSAY BY SPECTROPHOTOMETER

Solvent: ACN: Water, 1: 1, add equal amount of ACN and water.

SAMPLE PREPARATION:
TEXT TECHNICAL
Accurately weigh powder 0.33g equivalent to 20mg 0.33 g 100 mL
of Xegtin 20mg capsule in 100mL volumetric flask.
Make up volume with ACN: Water. Take 10mL of 10 mL 100 mL
above solution in 100mL volumetric flask and make
up volume with the same solvent. Measure the ʎ= 333 nm
absorbance at 333nm.

STANDARD PREPARATION:
TEXT TECHNICAL
Accurately weigh Piroxicam 0.191g equivalent to 0.191 g 100 mL
20mg of Piroxicam RS in 100mL volumetric flask.
Make up volume with ACN: Water. Take 10mL of 10 mL 100 mL
above solution in 100mL volumetric flask and make
up volume with the same solvent. Measure the ʎ= 333nm
absorbance at 333nm.
OBSERVATION AND CALCULATIONS

%age = ABSORBANCE OF SAMPLE X 100

ABSORBANCE OF STANDARD

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

7.3.3 DISSOLUTION:
Medium: Water: 900mL

RPM: 75 rpm

Time: 45 min

SAMPLE PREPARATION:
TEXT TECHNICAL
Add one capsule in each basket, volume of 900mL 1 capsule 900mL
water. Filter through 0.45-µm filter. Take 8mL of sample
(water)
from filtrate and dilute in 50 mL of water. Measure the
absorbance at 333 nm. Filter (0.45µm) ʎ= 333 nm

STANDARD PREPARATION:
TEXT TECHNICAL
Dissolve 0.191g of Piroxicam equivalent to 20mg of 0.191g 100 mL
Piroxicam RS in 100mL volumetric flask and makeup
volume upto 100mL with water. And take 1 mL and 10 mL 100mL
dilute with 100mL of water. Measure the absorbance at ʎ = 333 nm
333nm.

4
 SN/QC/SAPP/015
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 1 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE XEGTIN 20MG CAPSULES
Procedure: Determine the amount of PIROXICAM dissolved from UV absorbance at the wavelength of maximum
absorbance at about 333nm of suitable filtered portion of the solution under test. Suitably dilute with dissolution
medium, if necessary in compression with a standard solution having a known concentration of PIROXICAM in
the same medium.
Observation and calculations:
%age = ABSORBANCE OF SAMPLE X FACTOR OF STANDARD X 100
ABSORBANCE OF STANDARD FACTOR OF SAMPLE

Tolerance: NLT 80% of the labeled amount of PIROXICAM dissolved in 45 mins.

Reference: United States Patent,
Patent No.: US 7, 700, 579 B2

7.3.4 ASSAY FOR CAPSULES:

SAMPLE PREPARATION:
TEXT TECHNICAL
Weigh 20 capsules accurately weigh powder 0.33g 0.33 g 100 mL
equivalent to 20mg of Xegtin 20mg capsule in
100mL volumetric flask. Make up volume with 10 mL 100 mL
ACN: Water. Take 10mL of above solution in
100mL volumetric flask and make up volume with ʎ= 358 nm
the same solvent. Measure the absorbance at
358nm.

STANDARD PREPARATION:
TEXT TECHNICAL
Accurately weigh powder of Piroxicam 0.191g 0.191 g 100 mL
equivalent to 20mg of Piroxicam RS in 100mL
volumetric flask. Make up volume with ACN: Water. 10 mL 100 mL
Take 10mL of above solution in 100mL volumetric
flask and make up volume with the same solvent. ʎ= 358 nm
Measure the absorbance at 358nm.

OBSERVATION AND CALCULATIONS

%age = ABSORBANCE OF SAMPLE X 100

ABSORBANCE OF STANDARD

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

8.0 DOCUMENTATION:
 Request for Analysis
 Certificate of Analysis
 Inprocess Register
 Instrument Log Books
 Batch Manufacturing Record

9.0 REFRENCE:
In-house specs.