SN/QC/SAPP/027

Department Quality Control Issue # 0 3

Section Quality Control Issue Date 0 1 - 2 0 2 0
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STANDARD ANALYTICAL PROCEDURE MONAZ 5MG TABLET
PROCEDURE FOR ANALYSIS OF
MONAZ 5MG TABLET
(MONTELUKAST SODIUM)
(USP Specs)
DRN 056391

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 15.01.20 HURRYAM ALL Addition of Technical section

WRITTEN BY QC OFFICER

REVIEWED BY SENIOR QC OFFICER

APPROVED BY QC MANAGER

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SN/QC/SAPP/027
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 1 - 2 0 2 0
THIS DOCUMENT IS NOT VALID WITHOUT SIGNATURES
STANDARD ANALYTICAL PROCEDURE MONAZ 5MG TABLET
CONTENTS

1.0 AMENDMENT ……………………………………………..… 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 ASSAY (AFTER MIXING)……………………….04

7.3.2 ASSAY (AFTER COMPRESSION)……......…..04

7.3.3 ASSAY BY HPLC ………………………….……..05

7.3.4 DISSOLUTION …………………………………..06

8.0 DOCUMENTATION ...………………………………...……...07

9.0 REFERENCE ……..............................................................07

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SN/QC/SAPP/027
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 1 - 2 0 2 0
THIS DOCUMENT IS NOT VALID WITHOUT SIGNATURES
STANDARD ANALYTICAL PROCEDURE MONAZ 5MG TABLET
2.0 PURPOSE

This document is established to define the method of analysis for incoming product Monaz 5mg tablets to
confirm its physical and chemical properties.

3.0 SCOPE

This procedure is applicable in the Quality Control Department for the analysis of Incoming Monaz 5mg tablets.

4.0 PROCEDURE

Collect the sample according to sampling procedure (sop number SN/QC/SOP/0 21) and analyze it according to
the standard analytical procedure.

5.0 RESPONSIBILITY:

ANALYST

MANAGER Q.C

6.0 PRODUCT SPECIFICATIONS

Sr. PARTICULARS AFTER MIXING AFTER AFTER BLISTERING/

# COMPRESSION FINISHED
1. Physical Appearance Light yellow color powder Light yellow color A yellow color tablet.
Core tablet.
2. Identification Must be positive for Montelukast
3. Average weight 190mg ± 2% - -
4. Friability - N.M.T 1.0% -
5. Hardness - N.L.T 4.0 Kg -
6. Diameter - 8.0mm + 0.5mm -
7. Thickness - 3.0 + 0.5 mm -
8. Content uniformity - 85 – 115%
9. Dissolution - NLT 70%
10. Assay Limit 90 –110%

7.0 TESTS

7.1 Instruments
a) Volumetric Flask
b) Beaker
c) Pipette 1ml, 2ml ,10ml
d) Electric Balance
e) Dissolution apparatus
f) Spectrophotometer
g) DT apparatus

7.2 Reagents/Chemicals
a) Distilled Water
b) Methanol
c) Ethanol
d) Sodium dodecyl sulphate

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SN/QC/SAPP/027
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Section Quality Control Issue Date 0 1 - 2 0 2 0
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STANDARD ANALYTICAL PROCEDURE MONAZ 5MG TABLET
7.3 Chemical Analysis

7.3.1 ASSAY BY SPECROPHOTOMETER (AFTER FINAL MIIXING):

SAMPLE PREPARATION:
TEXT TECHNICAL
Take sample 0.76g equivalent to 20mg of Montelukast 0.76g 100mL
in 100mL volumetric flask. Make up volume with
methanol. Sonicate for 5 to 10 minutes. Take 5mL and 5mL 100mL
dilute to 100mL with same solvent. Measure the
absorbance at 285nm with suitable spectrophotometer. ʎ = 285 nm

STANDARD PREPARATION:
TEXT TECHNICAL
Weigh accurately Montelukast sodium 0.0207g 0.0207g 100mL
equivalent to 20 mg Montelukast RS and dissolve in 100
mL of methanol. Sonicate for about 5 to 10 min. Then 5mL 100mL
take 5mL from the above solution and dissolve in 100
mL with the same solvent. Scan the solution at 285 nm. ʎ = 285 nm

OBSERVATIONS AND CALCULATIONS:

Absorbance of the sample at 285nm = X

Absorbance of the standard at 285nm = Y

%AGE = X / Y X 100 = Z%

LIMIT: 90.0 – 110%

7.3.2 ASSAY BY SPECROPHOTOMETER (CORE TABLETS/FINISHED PRODUCT):

SAMPLE PREPARATION:
TEXT TECHNICAL
Take 20 tablets and crush them to fine powder. Take 0.76g 100mL
sample 0.76g equivalent to 20mg of Montelukast in
100ml volumetric flask. Make up volume with methanol. 5mL 100mL
Sonicate for 5 to 10 minutes. Take 5ml and dilute to
100ml with same solvent. Measure the absorbance at ʎ = 285 nm
285nm with suitable spectrophotometer.

STANDARD PREPARATION:
TEXT TECHNICAL
Weigh accurately Montelukast sodium 0.0207g 0.0207g 100mL
equivalent to 20 mg Montelukast RS and dissolve in 100
mL of methanol. Sonicate for about 5 to 10 min. Then 5mL 100mL
take 5mL from the above solution and dissolve in 100
mL with the same solvent. Scan the solution at 285 nm. ʎ = 285 nm

OBSERVATIONS AND CALCULATIONS:

Absorbance of the sample at 285nm = X

Absorbance of the standard at 285nm = Y

%AGE = X / Y X 100 = Z%

LIMIT: 90.0 – 110%

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SN/QC/SAPP/027
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 1 - 2 0 2 0
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STANDARD ANALYTICAL PROCEDURE MONAZ 5MG TABLET
7.3.3 Assay by HPLC:
Chromatographic system:  
Mode: LC
Detector: UV 255 nm
Columns:
Guard: 3.0 mm x 4-mm; packing L11
Analytical: 4.6-mm × 10-cm; 3µm packing L11
Column temperature: 50
Flow rate: 1.5ml per minute.
Injection size: 20µl
Run time: 2 times the retention time of Montelukast

Diluent: Methanol and water (3:1)

Solution A: 0.2% (v/v) Triflouroacetic acid in water
Solution B: Methanol and acetonitrile (3:2)

Mobile phase: See Table 1.

Time (min) Solution A (%) Solution B (%)
0 48 52
5 45 55
12 45 55
22 25 75
23 25 75
25 48 52
30 48 52

STANDARD SOLUTION:
TEXT TECHNICAL
Weigh accurately Montelukast sodium 12.54g
equivalent to 330 mg Montelukast RS and dissolve in
1000 mL of diluent. Sonicate for about 60 min. 12.54g (Eqv. to 330mg) 1000mL
0.33mg/mL of USP Montelukast Dicyclohexylamina RS
in Diluent.

SAMPLE SOLUTION:
TEXT TECHNICAL
Nominally 0.25mg/mL of Montelukast prepared as
follows :
Transfer 10 Chewable tablets to a suitable volumetric 9.5g (Eqv. to 250mg) 1000mL
flask, add 75% of the flask volume of diluent, and
shake vigorously for 60 minutes. Dilute with diluent to
volume. Pass a portion of the resulting solution through
a suitable filter of 0.45µm pore size, discarding the first
mL of filtrate. Use the filtrate.
Percentage:
Calculate the percentage of the labeled amount of Montelukast (C33H36CINO3S) in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) x 100
rU = peak response from the Sample solution
rS = peak response from the Standard solution
CS = concentration of Montelukast in the Standard
solution (mg/mL)
CU = nominal concentration of Montelukast in
the Sample solution (mg/mL)
Molecular weight of Montelukast, 586.18
Mr1 = Molecular weight of Montelukast
dicyclohexylamine, 767.50
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SN/QC/SAPP/027
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 1 - 2 0 2 0
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STANDARD ANALYTICAL PROCEDURE MONAZ 5MG TABLET
Mr2 =
Acceptance criteria: 92.5%–107.5%

7.3.4 Dissolution:
Medium: 0.5% (w/v) Sodium dodecyl sulfate in water; 900 mL.
Apparatus 2: 50 rpm
Time: 20 min
Solution A: 0.2% (v/v) Trifluoroacetic acid in water
Solution B: 0.2% (v/v) Trifluoroacetic acid in acetonitrile
Mobile phase: Solution A and solution B (1:1)

Standard solution:
TEXT TECHNICAL
Weigh accurately Montelukast sodium 0.0207g 0.0207g(Eqv. to 20mg) 100 mL
equivalent to 20 mg Montelukast RS and dissolve in
100 mL of methanol. Sonicate for about 5 to 10 min. 5.5 mL 100 mL
Then take 5.5mL from the above solution and dissolve
in 100 mL with the same solvent.

Sample solution:
TEXT TECHNICAL
Take sample 0.76g equivalent to 20mg of Montelukast 0.76g 100mL
in 100mL volumetric flask. Make up volume with
methanol. Sonicate for 5 to 10 minutes. Take 5.5mL 5.5mL
and dilute to 100mL with same solvent. 100mL

Chromatographic system:  
Mode: LC
Detector: UV 389 nm
Columns: 3.0 mm x 10-cm; packing L11
Analytical: 4.6-mm × 10-cm; 3µm packing L11
Column temperature: 50
Flow rate: 0.9ml per minute.
Injection size: 20µl
Run time: 1.5 times the retention time of Montelukast.

Percentage:
Calculate the percentage of the labeled amount of Montelukast (C33H36CINO3S) in the portion of Tablets taken:

Result = (rU/rS) × CS ×
V × (1/L) x 100
rU = peak response from the Sample solution
rS = peak response from the Standard solution
CS = concentration of Montelukast in the Standard
solution (mg/mL)
V = volume of Medium, 900Ml
L = label claim (mg/Tablet)
Tolerances: NLT 80% (Q) of the labeled amount of montelukast (C33H36CINO3S) dissolved.

8.0 DOCUMENTATION

 Request for Analysis

 Certificate of Analysis
 Inprocess Register
 Instrument Log Books

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SN/QC/SAPP/027
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 0 1 - 2 0 2 0
THIS DOCUMENT IS NOT VALID WITHOUT SIGNATURES
STANDARD ANALYTICAL PROCEDURE MONAZ 5MG TABLET
9.0 REFERENCE

USP 40: Volume 5. Page 5225