S SHAWAN

SN/QC/SAPP/007 Pharmaceuticals
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 7 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE SHAEZ 20MG CAPSULE

PROCEDURE FOR ANALYSIS OF

SHAEZ 20MG CAPSULE
(USP SPECIFICATIONS)

AMENDMENT SHEET

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
03 05.03.2020 ANEELA ALL Addition of Technical section

WRITTEN BY QC OFFICER

REVIEWED BY SENIOR QC OFFICER

APPROVED BY QC MANAGER

1
 S SHAWAN
SN/QC/SAPP/007 Pharmaceuticals
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 7 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE SHAEZ 20MG CAPSULE

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 ………………………………………… 04

7.3 CHEMICAL ANALYSIS…………………………….. 04

7.3.1 ASSAY FOR PELLETS…………………………………… 04

7.3.2 ASSAY BY SPECTROPHOTOMETER…………… 04

7.3.3. HPLC METHOD.……………………………………….... 05

7.3.4 DISSOLUTION.…………………………….…….... 06

8.0 DOCUMENTATION …………………………………………… 08

9.0 DISTRIBUTION …..…………………………………………… 08

10.0 REFERENCE …………………………………………………… 08

2
 S SHAWAN
SN/QC/SAPP/007 Pharmaceuticals
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 7 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE SHAEZ 20MG CAPSULE

2.0 PURPOSE:

This document defines the method of analysis raw material Shaez 20mg to confirm its physical and chemical
properties.

3.0 SCOPE:

This procedure is applicable in the Quality Control Department for the analysis of Shaez 20mg 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
Q.A OFFICER
MANAGER Q.C
QA MANAGER

6.0 RAW MATERIAL SPECIFICATIONS:

Sr. Particulars After Filling After Blistering

#
1. Physical Appearance P/Blue Color Filled Capsules. P/Blue Color Filled Capsules.

2. Identification Must be positive

for Esomeprazole
3. Disintegration Time(Shell) N.M.T 15 min

4. Content Wt/Caps 345mg/Capsule + 2% 345mg/Caps + 2%

5. Dissolution Acidic Stage….. NMT 10%

Buffer Stage……NLT 75%
6. Assay Limit 90 –110%

7.0 TESTS

7.1 Instruments
a. Beaker
b. Pipette
c. Flasks
d. Analytical Balance
e. Moisture analyze
f. Spectrophotometer
g. Dissolution Apparatus

3
 S SHAWAN
SN/QC/SAPP/007 Pharmaceuticals
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 7 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE SHAEZ 20MG CAPSULE
7.2 Reagents/Chemicals
a. Distilled Water
b. Acetonitrile
c. Methanol
d. Ethanol
e. Phosphate Buffer pH 6.8
f. Monobasic Sodium Phosphate
g. Dibasic Sodium Phosphate
h. Tribasic sodium phosphate dodecahydrate

7.3 Chemical Analysis

7.3.1 Assay By Spectrophotometer:

Sample Preparation:
TEXT TECHNICAL
Weigh accurately 0.088g pellets equivalent to 20mg
of Esomeprazole pellets to a 100 mL volumetric 0.088g 100mL (0.1N
flask. Dilute with 0.1N NaOH. Sonicate for 5 – 10 NaOH)
minutes. Take 5 mL from the above solution and
dilute to 100 mL with same solvent (0.01mg/mL). 5mL 100mL (0.1N
Measure the absorbance at 302 nm. NaOH)

ʎ = 302nm

Standard Preparation:
TEXT TECHNICAL
Weigh accurately 0.0223g Esomeprazole
Magnesium Trihydrate equivalent to 20mg (WS) to a 0.0223g 100mL (0.1N
100 mL volumetric flask. Dilute with 0.1N NaOH. NaOH)
Sonicate for 5 – 10 minutes. Take 5 mL from the
above solution and dilute to 100 mL with same 5mL 100mL (0.1N
solvent (0.01mg/mL). Measure the absorbance at NaOH)
302 nm.
ʎ = 302nm

Observation And Calculations

%Age = Absorbance Of Sample X 100
Absorbance Of Standard
LIMIT: 90.0% - 110.0%

7.3.2 Assay By Spectrophotometer For Capsules (Final Product):

Sample Preparation:
TEXT TECHNICAL
Take 20 capsules and remove complete content from 0.088g 100mL
the capsules and weigh accurately 0.088g of pellet
equivalent to 20mg of Esomeprazole and transfer to a 5mL 100mL
100mL volumetric flask, make volume to 100mL with
0.1N NaOH. ʎ = 302nm
Take 5 mL and dilute to 100 mL with same solvent.
Measure the absorbance at 302 nm.

Standard Preparation:
TEXT TECHNICAL

4
 S SHAWAN
SN/QC/SAPP/007 Pharmaceuticals
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 7 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE SHAEZ 20MG CAPSULE
Weigh accurately 0.0223g Esomeprazole Magnesium
Trihydrate equivalent to 20mg (WS) to a 100 mL 5mL 100mL
volumetric flask. Dilute with 0.1N NaOH. Sonicate for
5 – 10 minutes. Take 5 mL from the above solution ʎ = 302nm
and dilute to 100 mL with same solvent (0.01mg/mL).
Measure the absorbance at 302 nm.

Observation And Calculations

%age = Absorbance Of Sample X 100

Absorbance Of Standard
LIMIT: 90.0% - 110.0%

7.3.3 Assay by HPLC:

Chromatographic system:
Mode: LC
Detector: UV 302 nm
Column: 4.6-mm × 15-cm; 5 µm packing L7.
Flow rate: 1 mL/min
Injection size: 20 µL

Buffer: Prepare a pH 7.3 phosphate buffer by mixing 10.5mL of 1M monobasic sodium phosphate buffer
and 60mL of 0.5M dibasic sodium phosphate buffer, and diluting with water to 1000mL. Adjust pH with
NaOH or HCl.
Diluent: Prepare a pH 11.0 diluent as follows. Dissolve 5.24g of tribasic sodium phosphate dodecahydrate
in water. Add 110mL of 0.5M dibasic sodium phosphate solution and dilute with water to 1000mL. Adjust
pH with NaOH or HCl.
Mobile phase: Mix 350mL of Acetonitrile and 500mL of the Buffer. Dilute with water to 1000mL.

Standard preparation—
TEXT TECHNICAL
Transfer 10 mg of USP Omeprazole RS, accurately
weighed, to a 250-mL volumetric flask, and dissolve in 10mg 250mL (10mL
about 10 mL of alcohol. Add 40 mL of diluent and dilute alcohol+40mL diluent) (Water)
with water to volume. This solution contains 0.04mg/mL
of USP Omeprazole RS.
 
Sample Stock Solution:
TEXT TECHNICAL
Mix the content of NLT 20 capsules. Transfer a portion
of the capsules content, equivalent to 20mg of
Esomeprazole to a 100mL volumetric flask, add 60mL 20mg 100mL (60mL
of diluent and shake for 20mins to dissolve the pallets. diluent+20mL alcohol) (Diluent)
Sonicate for a few min, if needed to completely
dissolve. Add 20mL of alcohol and sonicate for a few
min. Cool and dilute with diluent to volume. Pass a
portion of the solution through a filter of 1µm pore size.

Sample preparation:
TEXT TECHNICAL
0.04mg/mL Esomeprazole from sample stock solution 4mL (Sample stock solution) 100mL

5
 S SHAWAN
SN/QC/SAPP/007 Pharmaceuticals
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 7 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE SHAEZ 20MG CAPSULE
in water. Store this solution protected from light. (Water)

Procedure— Separately inject equal volumes of the Standard preparation and the Assay preparation into

the chromatograph, record the chromatograms for about 30 minutes, and measure the responses for the
major peaks. Calculate the percentage of in the portion of Esomeprazole taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response from the Sample solution
rS = peak response from the Standard solution
CS = concentration of omeprazole in the Standard solution (mg/mL)
CU = concentration of Esomeprazole in the Sample solution (mg/mL)

LIMIT: 90.0% - 110%

7.3.4 Dissolution:

Acid Resistance Stage

Acid stage medium: 0.1 N hydrochloric acid; 300 mL.
Apparatus 2: 100 rpm.
Time: 02 hours.

Sample Preparation:
TEXT TECHNICAL
Add one capsule in each basket, volume of 300mL
0.1N HCl, and withdraw 30mL sample after 2 hours 0.088g 300mL 0.1N HCl
from the basket. Transfer 30mL sample in 100mL of
volumetric flask. And makeup volume with buffer
having pH 6.8. 30mL 100mL (buffer)
Then proceed immediately as directed for Test
solution in the Buffer stage. Determine the amount
of Esomeprazole dissolved by employing UV Filter (0.45µm)
absorption at the wavelength of maximum
absorbance at 302 nm, using Buffer stage medium
ʎ= 302 nm
as the blank.
Filter through 0.45-µm filter.

Standard Solution:
TEXT TECHNICAL
Weigh accurately 0.0223g Esomeprazole
Magnesium Trihydrate equivalent to 20mg (WS) to a
0.0223 g 100mL
100 mL volumetric flask. Dilute with ethanol.
Sonicate for 5 – 10 minutes. Take 10 mL from the (ethanol)
above solution and dilute to 100 mL with buffer
10mL 100mL (buffer)
(0.02mg/mL). Measure the absorbance at 302 nm.
ʎ = 302 nm

OBSERVATION AND CALCULATIONS

%age = Absorbance Of Sample X 100

Absorbance Of Standard
Tolerances: Not more than 10% of the labeled amount of Esomeprazole is dissolved in 2 hours.
Buffer Stage:
Medium: 0.086M dibasic sodium phosphate (12.212g dibasic sodium phosphate in 1000mL of distilled water) and
adjust with 2N HCl or 2N NaOH, if necessary to a pH of 6.8 ± 0.05, 700mL
Apparatus 2: 100 rpm.
Time: 30 minutes
6
 S SHAWAN
SN/QC/SAPP/007 Pharmaceuticals
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 7 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE SHAEZ 20MG CAPSULE
Sample Preparation:
TEXT TECHNICAL
After 2 hours for acid stage, add 700mL of the
buffer medium, and continue the test for 30 more 0.088g 1000mL (Buffer)
minutes with total 1000mL medium in each basket.
Take 100mL of sample from each basket. Filter
through 0.45-µm filter. Determine the amount of Filter (0.45µm)
Esomeprazole dissolved in filtered portions of the
ʎ = 302nm
Test solution, using the difference between the
absorbance at the wavelengths of 302 nm.

Standard Solution:
TEXT TECHNICAL
Weigh accurately 0.0223g Esomeprazole
Magnesium Trihydrate equivalent to 20mg (WS) to a
0.0223 g 100mL
100 mL volumetric flask. Dilute with ethanol.
Sonicate for 5 – 10 minutes. Take 10 mL from the (ethanol)
above solution and dilute to 100 mL with buffer
10mL 100mL (buffer)
(0.02mg/mL). Measure the absorbance at 302 nm.
ʎ = 302 nm

OBSERVATION AND CALCULATIONS

%age = Absorbance Of Sample X 100

Absorbance Of Standard
Tolerances: Not less than 75% of the labeled amount of Esomeprazole is dissolved in 30 minutes.

Dissolution By Hplc:

Mobile phase: Mix 350 mL of acetonitrile and 500 mL of the Buffer. Dilute with water to 1000 mL.
0.25M NaOH: 10g of Sodium hydroxide in 1000mL of distilled water.

Standard solution:
TEXT TECHNICAL
Prepare a solution containing 2 mg/mL of USP
Omeprazole RS in alcohol. Dilute this solution with pH 0.0223g 100mL(Alcohol)
6.8 phosphate buffer to obtain a solution containing 1mL 100mL(Buffer)
(L/1000) mg/mL, where L is the label claim, in 10mL 12mL (2mL of 0.25M
mg/Capsule. Immediately add 2.0 mL of 0.25M sodium hydroxide)
sodium hydroxide to 10.0 mL of this solution, and mix.

Sample solution: (Acidic Stage)

TEXT TECHNICAL
Add one capsule in each basket, volume of 300mL
0.1N HCl, dissolve 0.088g of Esomeprazole pellets
(one capsule) in 300 mL of 0.1N HCl, and withdraw 20mg 300mL (0.1N HCl)
30mL sample after 2 hours from the basket. Transfer
2.5mL sample in 10mL of volumetric flask. And
makeup volume upto 10mL with buffer having pH 6.8. 2.5mL 10mL (Buffer)
Then proceed immediately as directed for Test
solution in the Buffer stage. Determine the amount of
Esomeprazole dissolved by employing UV absorption
at the wavelength of maximum absorbance at about
302 nm, using Acid stage medium as the blank.
Filter through 0.45-µm filter.
7
 S SHAWAN
SN/QC/SAPP/007 Pharmaceuticals
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 7 - 2 0 2 0
STANDARD ANALYTICAL PROCEDURE SHAEZ 20MG CAPSULE

Sample solution: (Buffer Stage)

TEXT TECHNICAL
After 2 hours, add 700mL of the buffer medium, and
continue the test for 30 more minutes with total
1000mL medium in each basket. Filter through 0.45- 20mg 1000mL
µm filter. Take 8mL of sample from filtrate and
dissolve in 10mL buffer. Determine the amount of
Esomeprazole dissolved in filtered portions of the 8mL 10mL (Buffer)
Test solution

Mode: LC
Detector: UV 302 nm Sample
Column: 4.6-mm × 15-cm; 5-μm packing L1
Flow rate: 1 mL/min
Injection size: 20 μL

Calculate the percentage of Esomeprazole (C17H19N3O3S)

Result = (rU/rS) × (CS/L) × V × 100

rU = peak response from the Sample solution

rS = peak response from the Standard solution
CS = concentration of the Standard solution
L = label claim (mg/Capsule) to volume.
V = volume of Medium,

Tolerances:
Stage 1: NMT 10% (Q) of the labeled amount of Esomeprazole (C17H19N3O3S) is dissolved.

Stage 2: NLT 75% (Q) of the labeled amount of Esomeprazole (C17H19N3O3S) is dissolved.

8.0 DOCUMENTATION

 Request for Analysis (QR/QC/R 029)

 Certificate of Analysis (QR/QC/R 001)
 Inprocess Register (QRF/QC/054)
 Instrument Log Books
 Batch Manufacturing Record (SN/BMR/CAPSULE)

9.0 DISTRIBUTION:

Master File.
Quality Control Manager.
Quality Control Analyst.
10.0 REFERENCE:

USP 40. Volume 4, Page 4059