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Mr*dp"., V*nara, Mouchak, kaliakoir, Gazipur

Document Title: Process validation Final Report of Asmatab Tablet

DocumentNumber : VPL-PVFR-010
Document Type : Concurrent Validation

Signature
Io'cl'lV
Farhana Sultana Md Tarikul Islam Bossunia Md. Moniruzzaman
PD Officer Asst. Manager, QualitY Control A Manager

COMPANY PROPRIETARY AND CONFIDENTIAL

 Frocess Validation
Veritas Pharmaceuticals limited VPL-PVFR.OO9
Muradpur,Vannara,Mouchak,GaziPur Rev No.:00

TABLE OF CONTENT

Validation team
personnel
Qualification and training of
Culib.ution and qualihcation status of equipment

Qualifi cation of starting materials

D.t"ilt of reference / working standards

Validation parameter, sampling & testing pian, results and acceptance

criteria for QualitY Control
Deviation rePorting
Review of results and rePorting

Final approval

COMPANY PROPRIETARY AND CONFIDENTIAL

Fage 1 of I
Asmatab Tablet
 Veritas Pharmaceuticals limited Frocess Validation
VPL-PVFR-O09
Muradpur,Vannara, Mouchak,GaziPur
Rev No.:00

tr 1.0 Introduction
This repofi includes the process validation activities for the manufacture of Asmatab Tablet.

2.0 Purpose
raw
The objective of the Performance Qualification report is to verif' that the manufacturing equipment'
material and the manufacturing & coating process for Asmatab Tablet specified in SPEC/BD 001/FP/O1
produces a tablet product of tn. consistent strength, weight, Hardness, Dissolution, Thickness,
Disintegration and water content.

3.0 Scope

This reporl is valid for Performance Qualification of Concurrent Validation for Asmatab Tablet at
manufacturing facility of VPL, Gazipur"

4.0 Qualification and training of personnel

personnel engaged in the Validation project have adequate qualification and are trained in the basic
principles of ,uiidutio, and thoroughly briefed about the manufacturing process of Asrnatab Tablet and
ih. d.tuil.d methodoiogy to be adopted for the Performance Qualifieation of the process.
A list of fhe nersonnel with the qualificat on and training details is AS n forrnat:
1 he following

Name Designation Department Signature of Signature of

Trainee Trainer
r-^'f" ll\rr&.
Farhana Sultana PD Officer Product Development
Executive, QC Oualitv Control Vt'tr<V boar
Md. Moniur Rahman
Md. Shafavat Hossain Sr. Executive. PD Product Development a gA a.ih// Ba,
Md. Mehedi Hasan Plod. Officer Production .( $Lwze:
Md. Abul Fazal Prod. Officer Production illYd- W
Md. Shahedul Islam OA Officer Oualitv Assurance rV/""- bhct*
5"0 Calibration and qualification status of equipment
The calibration and qualification status of the following equipments used in thq Performance
rralification of orocess Asmatab Tablet are checked and listed in the fbllowing t'olrng!
Equipment Name Identification No. Qualifi cation Reference Status
No:
Disintegration Tester oc-DT-O8 vPL-QC-002-00 Calibrated
Friabilitv Tester oc-FT-11 vPL-QC-004-00 Calibrated
Karl Fisher Titrator oc-KF-23 vPL-OC-020-00 Calibrated
Slide Caliper (Disital) oc-sc-17 vPr.-oc-021-00 Calibrated
Dissolution Tester oc-DS-06 vPL-OC-003-00 Calibrated
Hardness tester oc-HT-O7 vPL-QC-oo5-00 Calibrated
Analvtical baldnce oc-AB-18 VPL-OC-001-00 Calibrated
HPLC oc-LC-01 vPL-OC-012-00 Calibrated

7.0 Qualification of starting materials

All the raw materials proposed to be used for the manufacture of validation batches have the following
qualification.
1) They comply with the relevant pharmacopoial specifications'
2) Tfe same batch number active principle are used for all the validation batches.
8.0 Details of reference / working standards

Sl. No. Name Source Streneth Exo. Date

0l Montelukast Sodium Morepen Lab Ltd. India 98.80 % (As is) Iulv.2014

Asmatab Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 2 of 8

 Process Validation
Veritas Pharmaceuticals limited VPL.PVFR-OOg
Muradpur,Vannara, Mouchak,Gazipur
Rev No.:00

t, Control
9.0 validation parameter, sampling & testing plan, results and acceptance criteria for Quality

PROCESS VALIDATION OF BLENDING STAGE

Results Mean Acceptance Remarks

Parameters Batch Samples in each
number stage criteria
Top-i 2.45 2.53 Complies
os-12
Top-2 2.56
Middle-l 2.65
Middle-2 2.48
Bottom-l 2.35
Bottom-2 2.67
Top-1 1.22 Complies
AS-04 12
Top-2 t3 Average
Moisture Middle-i 1.15 moisture content
Content bv KF Middle-2 is not more than
35
(%w/w) 3.s%
Bottom-l -'t 1+

Bottom-2 22
Top-1 1.50 Complies
3t2021 56
Top-2 5

Middle-1 45
Middle-2 1.43
Bottom-1 r.63
Bottom-2 t.43

Composite Results Acceptance Remarks

Parameter Batch
No. Ranse Mean RSD criteria
9"85 9"79 0.s3 Complies
os-12 Top-1
Top-2 9.82
Middle-1 9.84
Middle-2 9.78
Bottom-1 9.72
Bottom-2 9.75
Top-1 10.01 9"91 0.57 Complies
AS-04
Content of Too-2 9.91 9.00 - 11.00

Montelukast Middle-1 9.87

( mg/Tab) Middle-2 9.86
Rottom-1 9.87
Bottom-2 9.92
312021 Top- I 9.89 9.89 1.12 Complies
Ton-2 9.88
Middle-1 10.09
Middle-2 9.85
Rottom-1 9.84
Rottom-2 9.76

Asmatab Tablet COMPANY PROPRIETARY AND CONFI DENTIAL Page 3 of B

Veritas Pharmaceuticals limited Frocess Validation
Muradpur,Vannara,Mouchak,Gazipur VPL-PVFR-OO9
Rev No.:00

PROCESS VALIDATION OF COMPRESSION STAGE

Parameter Batch no. Acceptance Criteria Remarks

os-12 A white to off-white colored, round shaped White to offl-white colored,
AS-04 tablet with "V" engraved on one side and round shaped tablet with "V"
Description engraved on one side and break
312021 break line on other side.
line on other side.

Parameter

Complies
Avg. wt.:90.25
rng - 99.75 rng
20 tablets of (95.0 mg + 5%)
Middle

Uniformity of
wt.: Out of 20
Tablets
maximum 2
Uniformity 20 tablets of tablets shall
of mass
Middle deviate * 7 .5Ya
of average
weight and none
shall deviate +
312021
15%o ofaverage
*tt*n'
20 tablets of ,
Middle

Parameter Batch Composite Results Acceptance Remarks

No. Ranse Mean RSD criteria
os-12 10 tablets 96.8 - 97.86 0.84 Complies
99.1

Content
AS-04 0 tablets 96.1 98.54 t.12
uniformity I
(8s-1 1s)%
100.2
of of the label claim
Montelukast
(%) 312021 I 0 tablets 96.7 - 98.44 1.21
100.5

Asmatab Tablet COMPANY PROPRIETARY AND CONPI DENTIAL Page 4 of 8

Veritas Pharmaceuticals limited Frocess Validation
Muradpur,Vannara, Mouchak,Gazipur VPL-PVFR-OO9
Rev No.:00

Parameters Batch number Samples in each Results Acceptance Remarks

stase criteria
os-12 0 tablets of Top 3.02 3 5 Complies
0 tablets of Middle 3.0s 3 8

0 tablets of Bottom 3.42 - 3 3

Thickness AS-04 0 tablets of Top 3.06 - 3 7 2.90 mm - Complies

(mm) 0 tab ets of Middle 3.05 - 3 2 3.25 mm (3.10
0 tab ets of Bottom 3.02 3 J mrn + 5olo)
312021 0 tab ets of Top 3.03 - 3 5 Cornplies
0 tablets of Middle 3.05 -3 2
t0 tablets of Bottom 3.02 - 3 .16
os-12 6 tablets of Top 4.0 Complies
6 tablets of Middle 4.2

6 tablets of Bottorr 4.1

AS-04 6 tablets of Top 4.3 Complies

Average
6 tablets of Middle 4.2 .I
Disintegration NMT 5 min
Time 6 tablets of Bottom 4.5

312021 6 tablets of Top 4.7 Complies

6 tablets of Middle 4.8

6 tablets of Bottom 4.8

os-12 4.8 Complies

10 tablets of Top

10 tablets of Middle 4.9

I0 tablets of Bottom 4.6

Average AS-04 10 tablets of Top 4.7 Complies

Not less than
Hardness (Kp) 4.7
10 tablets of Middle 3.5

10 tablets of Bottom 4.6

312021 10 tablets of Top 4.7 Complies
l0 tablets of Middle 4.8

10 tablets of Bottom 4.5

os-i2 Top 0.02 Complies

Middle 0.03

Bottom 0.02

AS-04 Top 0.12 Complies

Friabilitv, (%o)
0.1
Middle 1
NMT 1.0%
Bottorn 0.12
3t2021 Top 0.12 Complies

Middle 0.1I

Bottom 0.15

Asmatab Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 5 of B

 Veritas Pharmaceuticals limited Frocess Validation
Muradpur,Vannara, Mouchak,Gazipur VPL-PVFR-OO9
Rev No.:00
,/t
i PROCESS VALIDATION OT' COATING STAGE

Parameter Batch no. Acceptance Criteria Remarks

os-12 A white to Off white colored, round white to Off white colored, round
AS-04 shaped film coated tablet with "V" shaped film coated tablet with "V"
Description
31202t engraved on one side and other side engraved on one side and other side
break line" break line"

Parameter Batch No. Sample in Results Acceptance Remarks

each stage Range Mean o/
/o criteria
variation
os-t 2 20 tablets 93.2 - 96.2 - J.IJ Complies
ofTop 98.4 +2.27
Avg. wt.:92^0
20 tablets 92.s 95.9 -3.58
of 99.1 +3.30
mg - 102.0 mg
Middle (97.0 mg * 5
20 tablets 92.6 - 96.1 -3.62 %)
of Bottom 98.1 +2"11
AS-04 20 tablets 94.5 -99.4 97.7 -J.JJ
ofTop +1.71
Uniformity 20 tablets 93.4 - 97.8 -4.53 Uniformity of
of mass of Middle 99.3 +1.50 wt.: Out of 20
Tablets
20 tablets 93.8 - 97.7 -3.98
maximum 2
of Bottom 99.6 +i.96
tablets shall
312021 20 tablets 93.4 - 97.6 -4.33 deviate +7.5Ya
ofTop 99.2 +1.61 'ofaverage
20 tablets 94.5 - 97.6 -3.16 weight and none
of Middle 99.1 +1.56 shall deviate +
15oZ of average
20 tablets 94.5 - 97.8 -3.35 weight
of Bottom 99.8 +2.07

Asmatab Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 6 of B

 Veritas Pharmaceuticals Iimited
Muradpur,Vannara,Mouchak,Gazipur Process Validation
VPL-PVFR-OO9
Rev No.:00
Parameters Batch number Samples in each Results Acceptance Remarks
stage criteria
os-12 10 tablets of Top 3.11- 3.20 Complies
l0 tablets of Middle 3.09 - 3.24

l0 tablets of Bottom 3
- 3.23
.14
AS-04 l0 tablets of Top 3.14 - 3.22
Thickness (mm) 3.0 mrn - 3.33 Complies
10 tablets of Middle 3.05 - 3.21 mrn (3.17 rnm
l0 tablets of Bottom 3.12 - 3 .25
* s%)
312021 l0 tablets of Top 3.10 - 3 .26 Complies
l0 tablets of Middle 3 .12
- 3.26
10 tablets of Bottom 3.11- 3.27
os-12 6 tablets of Top 5.1 Complies
6 tablets of Middle 5.2

6 tablets of Bottom 5.1

AS-04 6 tablets of Top
Average 7.9 Complies
Disintegration 6 tablets of Middle 7.9
Time NMT 30 rnin
6 tablets of Bottom 8.0
312021
6 tablets of Top 6.0 Complies
6 tablets of Middle 6.2

6 tablets of Bottom 6.1

u5-tz 5.3
10 tablets of Top Complies

l0 tablets of Middle 5.3

l0 tablets olBottom 5.4

Average AS-04
I0 tablets of Top 5.4 Complies
Ilardness (Kp)
l0 tablets of Middle 5.3 Not less than 4

l0 tablets of Bottom 5.2

312021 10 tablets of Top ).J Complies
10 tablets of Middle 5.4
l0 tablets of Bottom 5.5
os-12 Composite 84.9% Complies

Dissolution AS.O4
(7o Release Composite 9l.goh Not less than
Complies
of Montelukast) 70Yo within 45
312021 minutes
Composite 91.5yo
Complies

Asmatab Tablet
COMPANY PROPRIETARY AND CONFIDENTIAL
Page 7 of B
 Veritas Pharmaceuticals limited
Muradpur,Vannara, Mouchak,Gazipur Process Validation
VPL-PVFR-OO9
Rev No.:00

1O.O DEVTATION REPORTING

After careful study ofall results no deviation found.

11.0 REVIEW OF RESULTS AND REPORTTNG

Results collected from the three batches are reviewed

and a validation repoft is prepared.

FNAL SUMMARY REPORT

Final Summary repoft with conclusion and recommendation
are included in validation report.

COMPILATION OF CONTROL DATA AND RECORDS

control data and records ofthree batches is compiled and
compliance to be checked as per validation protocol
and its acceptance criteria.

BATCHANALYSIS R.EPORT
Finished batch analysis report of three batches is
compiled and Uniformity and RSD to be checked
parameter for compliance. for each

12.0 FINAL APPROVAL

Product : Asmatab Tablet

I.o:est
Reference
:

;
_gianulati
VpL-pVp-0I0

Three batches, (OS-I2, AS-04 &

studied for Performance Qualification of concurrent

validation. Based on the satisfactory results of, process
parameters
and analytical tests, the process is quarified
in accordance with the protocol.
The product is approved for commercial

Prepared by:

PD Officer
Signature:
Date :

Checked by:

Asst. Manager, QC
,rrnurur",
Date :
%i*rJ
lhl^t /t)
Authorizcd by:

QA Manager
Slgnature:
_a+,r,r-
Date ,t0.01;f9--
cc: Head, Production
cc: Product Development

Asmatab Tablet COMPANY PRoP RI ETAR' AN D co|.jmEiliAl Page I of B