ANALYTICAT M ETH OD VALIDATION REPORT

Product Name Asmatab Tablet Page No. 1-of8

ffieritas (Montelukast 10 mg as Montelukait
Sodium INN)
Report No.: Method No. TPIBD 001/00 Test parameter Assay by HPLC
vPr/MVR-o14 Revision No. 00 Date Revised New

Analytical Method validation report for Asmatab Tablet.

Prepared bv: Checked bv: Aooroved bv:

Name Farhana Sultana Md. Tarikul lslam Bossunia Md. Moniruzzaman

Desionation PD Officer Asst. Manager, QQ QA Manaoer

Signature
F^tA,anq @v,-v,J'
Date Lq fo,tlltl L1/o b./ 14 L9 t oo-,1 l"t
 ANALYTICAT M ETH OD VALIDATION REPORT
Product Name Asmatab Tablet Page No. 2of8
ffieritas (Montelukast 10 mg as Montelukast
Sodium INN)
Report No.: Method No. TP/BD 00u00 Test parameter Assay by HPLC
vPr/MVR-o14 Revision No. 00 Date Revised New

TABTE OF CONTENTS
Serial No. Contents Page No.

1, Purpose 03

2 Objective 03

3 Scope 03
4 Materials, Reagent and Column 03
4.1 Primary material 03

4.2 Regents 03

4.3 Column 03

5 lnstrument Qualification 03

6 Methods Validation Analytical Performance characteristics To Be Evaluated 04

6.1 Accuracy o4
6.2 Precision o4
6.2.1 Repeatability (Method Precision) 04
6.2.2 lntermediate Precision 05

6.3 Linearity and range 05

6.4 Specificity 06
6.4.L Placebo effect 06
6.5 Sensitivity (LOD and LOQ) 06-07
6.6 System Suitability 07
7 Deviation 07
8 Report 07-08
9 Revision History 08

Md. Tarikul lslam Bossunia

 ANALYTICAL METHOD VALIDATION REPORT
Product Name Asmatab Tablet Page No. 3 of 8
$erl{as (Montelukast 10 mg as Montelukasi
Sodium INN)
Report No.: Method No. TPIBD 00u00 Test parameter Assay by HPLC
vPL/MVR-o14 Revision No. 00 Date Revised New

1. Purpose: The purpose of this report is to validate the analytical method for assay of Asmatab Tablet.

2. Objective: The objective of this report is to give the evidence of the validity of the method for assay of Asmatab Tablet.

3. Scope: To evaluate the acceptability of analytical method for its intended purpose. lt will define the procedure,
documentation, references and acceptance criteria to be used in the validation of assay method of Asmatab Tablet.
4. MATERIALS, REAGENT AND EQUIPMENTS
4.l PRIMARY MATERIAL
Sr. No. Name Source Descriotion
01 Asmatab Tablet Veritas Pharmaceuticals Ltd, Tvpe Finished Product
Bangladesh Batch No. 402003
Shelf life 03 years
o2 Montelukast Sodium Morepen Lab Ltd. lndia Tvoe Workine Standard
Batch No. MtT-3013
Shelf life July 2074

4.2 REAGENT
Sr. No. Reasent Name Manufacture Batch No. Shelf Life
01 Ammonium Acetate Sharlau, Spain 11934801 August 2015
02 Glacial Acetic Acid Active Fine Chemicals Ltd. BD GAAGR I2O5OO2 April2015
03 Methanol Active Fine Chemicals Ltd. BD Melhe 1307013 June 2016

4.3 Column
Sr. No. Description ID
01 Kromacil 100-C18 HD, l-50 x4.6 mm, 5p or Equivalent QCHC- 010

5. INSTRUM ENT QUALIFICATION

The below instruments should be used for this validation:

Sr. lnstrument Brief Description QAD No. Calibration Record Doc. No.
No. Name
01 HPLC . PerkinElmer Flexar QC-LC-o1 Date of Calibration 09.03.14 VPL/QC/QC-
HPLC integrated Next due date 08.04.14 LC-01/001
with PDA detector Calibration done by Md. Masud Rana
02 Analytical BOECO Electronic QC-AB-18 Date of Calibration 03.o2.t4 VPL/QC/QC-
Balance Balance Next due date 02.o8.74 AB-0u018
Calibration done by Md. Mizanur Rahman

Prepared bv: Checked bv: ADoroved bv:

Name Farhana Sultana Md. Tarikul lslam Bossunia Md. Moniruzzaman

Desionation PD Officer Asst. Manaqer, QC .r QA Manaqer

Signature (r.rt.-^-laA' $fto"
Fg,Yl',an,\
Date )qr0altu L21u 3/ q q.Yl\(, / IV
 ANATYTICAL M ETHOD VALIDATION REPORT
Product Name Asmatab Tablet Page No. 4of8
ffierltas (Montelukast 10 mg as Montelukast
Sodium INN)
Report No.: Method No. TPlBD 001/00 Test parameter Assay by HPLC
vPr/MVR-014 Revision No. 00 Date Revised New

6. METHODS VALIDATION ANATYTICAL PERFORMANCE CHARACTERISTICS TO BE EVATUATED

6.1 Accuracy

Added Recovery VIean

Sample Recovered )verall Mean
Label Sample Recovery% (%) Range lecovery(%) at
No, QtY(mg) n=9)
Qty(me) at each label :ach label
L 8.0 8.05 100.67 L00.50 - 100.88
80% 2 8.0 8.04 100.s0 101.48
3 7.9 8.O2 101.48
1 10.0 9.89 98.91 98.91- 99.6s
L00% 2 9.9 9.93 100.30 100.30
LOO.37
3 9.9 9.87 99.74
1 12.0 1.2.O5 100.38 100.29 - 100.58
120% 2 lt.9 12.03 701.07 101.07
3 L2.0 12.04 100.29
SD o.74
% RSD 0.74

Acceptance criteria: Average recovery at each level within 98% lo 102% and RSD value of nine determinations must
be less lhan 2%.
/
.(
Result: Complies 1 Not Complies
Data Attached

6.2 Precision
5.2.1 Repeatability (Method Precision)

Result:

o/o Av. Assay (o/o)

Sample No. Assay (n=6) STDEV RSDo/o

1 99.21
2 100.33
3 99.03
99.51 0.62 0.62
4 100.26
5 99.19
6 99.02

Acceptancp criteria: RSD of the active contents of six samples must be less than 2%.
/
Result: {Complies 1 Not Complies
Data Attached

Preoared bv: Checked bv: Aooroved bv:

Name Farhana Sultana Md. Tarikul lslam Bossunia Md. Moniruzzaman

Desionation PD Officer Asst. Manaoer, QC QA Manaqer

Signature lA{h&v\o\
'29/o<llLl
ffi:,;l't''"\ -Wv*-
Date 7-L)/0',)/14 cv)l n(, / lY
 ANALYTICAL METHOD VATIDATION REPORT
Product Name Asmatab Tablet Page No. 5of8
$ritas (Montelukast 10 mg as Montelukast
Sodium INN)
Report No.: Method No. TPIBD 001/00 Test parameter Assay by HPLC
vPr/MVR-o14 Revision No. 00 Date Revised New
5.2.2. lntermediate Precision

Analyst 1 Analyst 2
Done By Farhana Sultana Md. Mizanur Rahman
Location QC Lab QC Lab
lnstrumenl
Used HPLC HPLC
Date of
Analysis 27.O3.t4 28.03.14
Label spl Mean Label spl
Assay% STDEV RSD%
Mean
Claim% No. Assay% Assay% STDEV RSD%
Claimo/o No. Assay%
t 99.21 t 99.5
2 100,33 2 100.4
3 99.03 3 99.0
100 99.51 0.62 0.62 100
4 L00.26 99.61 0.72 0.72
4 98.9
5 99.19 5 99.1
6 99.O2 6 100.6
Acceptance criteria: RSD of the active contents of six samples must be less than 2yo.asper Repeatability day 1.
Remarks: iEl'Compl ies EI Not Complies
Data Attached

6.3 Linearity

%std Peak area of

Montelukast Linearity Study - Montelukast
60 950009.6 1500000
t! y=1E+07x+7658.
80 1240s97.6 o
1000000 R2 = 0.999
100 1.544646.5
l! 500000
1848953.4 o
120 CL

213238.0 0
140
0.05 0.1 0.15

Conc. Of Montelukast (mg/ml)

Montelukast
Acceptance criteria: The calibration curve should be linear (visually) and the value of R2 must be > 0.99
Remarks: Gomplies ElNot Complies

Prepared by: Ghect(ed by: Approved bv:

Name Farhana Sultana Md. Tarikul lslam Bossunia Md. Moniruzzaman

Desiqnation PD Officer Asst. Manager, Qc QA Manaoer

Signature
frilJr- d"Je'^
Date 4i01llq q$l o'\/l\
 ANALYTICAL METHOD VALIDATION REPORT
Product Name Asmatab Tablet Page No. 6of8
ffiritas (Montelukast 10 mg as Montelukast
Sodium INN)
Report No.: Method No. rPlBD 001/00 Test parameter Assay by HPLC
vPL/MVR-o14 Revision No. 00 Date Revised New

Range:

Used Range :80%-t2Q.O% of test concentration

Sl No. Parameters Result Limit

1 Accuracv % Montelukast 100.37 98.0%-102.0%

2 Precision RSD% for lntra Assav o.62 NMT 2.0%
RSD% for lntermediate Assay o.72 NMT 2.0%

3 Linearity Correlaion Coefficient R2 (Montelukast) 0.999 NLT 0.99

6.4 Specificity

5.4.1 Placebo effect

Retention Time Peak Area

Placebo 0.00 0.00

Blank 0.00 0.00
Standard 4.933 972070.5
Sample 4.9!9 996035.8
%lnterference by Blank or Placebo 0.00 0.00

Acceptance criteria: There will be no interference at the peak region of Montelukast due to Placebo/Blank
solution.
,/
Remarks: 'f Complies 'l Not Complies
Data Attached

6.5 Sensitivity

Conc. Average Peak Slope ofthe Intercept Residual 60000 Y=8Q22.x+7300.

(! R2 = 0.997
(ppm) Area.of Regression Standard 0,
L 40000
Montelukast line (S) Deviation
lt, 20000
(n:2) (o) 0,
CL

I 15748.9 8022 7726.1,5 737.0s 0

1 30s 17.8 6449.55 246
5 47839.9 7726.15
Of Montelukast (ppm)

Preoared bv: Checked bv: Aooroved bv:

Name Farhana Sultana Md. Tarikul lslam Bossunia Md. Moniruzzaman

Desionation PD Officer Asst. Manaqer. QC QA Manaqer

Signature (aftr-n^* ffii^*ayq
Date t-q I a>) 14 /-9/O1 ,/ t4' wtoq/tY
 ANATYTICAL METHOD VATIDATION REPORT
Product Name Asmatab Tablet Page No. 7 of I
ffir[tms (Montelukast 10 mg as Montelukast
Sodium INN)
Report No.: Method No. TPIBD 001/00 Test parameter Assay by HPLC
vPL/MVR-o14 Revision No. 00 Date Revised New

LOD = 3.3 o /s = 3.3 x737.05/8022 = 0.30 ppm

LOQ = 10 o /s = 10 x737.05/8022 = 0.92 ppm

6.6 System Suitability

lnjection
Tailing Factor Retention Time (min.) Area Theoretical Plate Count
No.
1 1.35 4.933 972070.5 1868
2 1.366 4.924 979045,8 1.904
3 1.36 4.922 974558.1 1902
4 1..376 4.922 974395,1 L920
5 1..376 4.920 973842.6 1905
6 L.372 4.933 9729s2.9 1915
Avg. (n = 6) 1.37 4.93 974477.5A 1902
% RSD 0.7s o.12 o.2s 0.96
Limit: NMT 2 RSD%: NMT 2.0% RSD%: NMT 2.0% NLT 15OO

./'
Remarks: VComplies 1 Not Complies
Data Attached

7. DEVIATION: No deviation"

Preoared bv: Checked bv: Aporoved bv:

Name Farhana Sultana Md. Tarikul lslam Bossunia Md. Moniruzzaman

Desiqnation PD Officer Asst. Manaqer, QC QA Manaqer

Signature (:av /.u,na' f4"
\"(4.M- l^^4
Date L7t0>t t4 )9/DZ,/ )4
 ANALYTICAL M ETHOD VALIDATION REPORT
Product Name Asmatab Tablet Page No. 8 of 8
ffirEtas (Montelukast 10 mg as Montelukast
Sodium INN)
Report No.: Method No. TPIBD 001/00 Test parameter Assay by HPLC
vPr/MVR-014 Revision No. 00 Date Revised New

8. REPORT

ment : Product
Product Name : Asmatab Tablet
Summary & Discussion ;

The data collected so far suggests that method is suitable and there is no significant change with respect to the established
limits.
Conclusion & Recommendation :

Based on this it is concluded that this method can be assiqned as Analvtical method for the assav of Asmatab Tablet.

Method is considered as validate.

[---l Method is not suitable.

Prepared by:
Signature : Furtwq
Date : 2s ta\ J lv1
Checked by:
Signature:
Date : Leri ,/n<,4a
Approved by:
Signature
Date

9. Revision History

Sl. No. Version & lssue details Revision/Change in brief Reason for change

7 Version : 00, Date of issue: Newly created. lnitial document

March 2014

Prepared bv: Checked bv: Approved bv:

Name Farhana Sultana Md. Tarikul lslam Bossunia Md. Moniruzzaman

Desionation PD Officer Asst. Manaqer, QC QA Manaoer

Signature
E"A*o. ffi{,-y^r1
Date ta lh.l I lL) 2n/a 3,/ la ry9 IOqt IV