GMH LABORATORIES

Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan

(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 1 of 18

PRODUCT: LEVOCETIRIZINE TABLETS IP

STANDARD BATCH SIZE: ……………..Tablets

REPORT No.: GMH/PVR/L05/23/01

VERSION No.: 01

EFFECTIVE DATE:

Format No.: QA-030/ A02/00

 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 2 of 18

TABLE OF CONTENTS
S. No. Page Nos.
TABLE OF CONTENTS
Cover Page 01 of 27

Table of contents 02 of 27

1.0 Product Details 03 of 27

04-05 of 27
2.0 Pre request for Process validation
05-06 of 27
3.0 Equipment & Machine List
07 of 27
4.0 Process validation Strategy
07-08 of 27
5.0 Approved Raw & Primary Packing Material
08- 23 of 27
6.0 Manufacturing Process
23-25 of 27
7.0 Packing
25 of 27
8.0 Final Result of finish product
26 of 27
9.0 Results Evaluation
26 of 27
10.0 Deviation
26 of 27
11.0 Stability
26 of 27
12.0 Abbreviation

13.0 Report approval sheet 27 of 27

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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 3 of 18

14.0 End of the Document 27 of 27

1.0 PRODUCT DETAILS:

Process validation of Levocetirizine
Generic Name : Levocetirizine Tablets IP

Standard Batch Size : 1,00,000 Tablets

Shelf Life : 24 Months
Average weight of tablets : 140 mg
Composition :
Each Uncoated tablet contains:
Levocetirizine Dihydrochloride IP 5 mg
Excipients q.s.

Description: White colored round shaped biconvex having plain on both side Film coated tablet.

Format No.: QA-030/ A02/00

 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 4 of 18

The quantity of various ingredients required for the manufacturing of the batch is detailed below.
SR.No Material Name Spec. Function Qty. Per Qty. For
. Tablet 1,00,000
(mg) (kg)
1. MCC Plain IP Binder 50.00 5.000

2. D.C.P IP Binder 30.00 3.000

3. Maize Starch IP Binder 20.00 2.000

4. Maize Starch IP Lubrication 4.00 0.400

5. PVPK-30 IP Lubrication 2.000 0.200

6. Purified Water IP Solvent q.s. 4.000

7. Levocetirizine IP Active 13.00 1.300

8. MCC-102 (DC Grade) IP Lubrication 5.250 0.525

9. Crosspovidone XL-10 IP Lubrication 3.000 0.300

10. Crosscarmellose Sodium IP Lubrication 4.000 0.400

11. Sodium Lauryal Sulphate IP Lubrication 1.000 0.100

12. Colloidal Silicon Dioxide IP Lubrication 2.000 0.200

13. Talcum IP Lubrication 6.000 0.600

14. Magnesium Stearate IP Lubrication 2.750 0.275

15. M.C.C -102(Excess) IP Lubrication 3.000 0.300

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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 5 of 18

2.0 PRE REQUEST FOR PROCESS VALIDATION

2.1 FACILITY DESIGN AND QUALIFICATION
The area where manufacturing of the Levocetirizine Tablets IP is proposed is evaluated for the
fitness and qualification status to manufacturing of product:
Sr. No. Unit Operation Manufacturi Manufacturing AHU
ng Area Condition Qualification
Name Report
Sifting, Granulation, Granulation Temperature:
1.
Drying & Sizing area NMT 25±2 ºC
2. Lubrication Blending Area RH: NMT 55 ± 5%
Compression Temperature:
3. Compression
Area NMT 25±2 ºC
Inspection RH: NMT 55 ± 5%
4. Inspection
Area
Temperature:
5. Alu-Alu Packing Packing
NMT 25±2 ºC
2.2 UTILITIES QUALIFICATION
The utility involved in the manufacturing shall be evaluated for its qualification.
Sr. No. Utilities Qualification Report no.
1. Purified water system
2. Compressed air system
2.3 EQUIPMENT QUALIFICATION
Sr. No. Equipment Name Equipment ID Qualification Protocol/ Report
No.
1. Rapid Mixer Granulator PD/RM/001
2. Fluidized Bed Dryer PD/FB/001
3. Octagonal Blender PD/OB/002
4. 27 Station Double Rotary
PD/CM/002
Tablet Compression machine
5. Auto coater PD/AC/001
6. Alu-Alu Packing Machine PD/AP/001
3.0 EQUIPMENTS AND MACHINE LIST
All the equipment and machines is checked for cleanliness prior of use and check for the status
label displayed. Equipment required for the process validation of Levocetirizine Tablets IP are
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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 6 of 18

as follows:

Sr. No. Equipment Capacity Equipment Id

600 gm, PD/WB/002
1 kg, WH/WB/003
Electronic Balances
1. 10 kg, WH/WB/002
150 kg, WH/WB/001
300 kg PD/WB/001
2. Vibro Sifter 100Kg/Hrs PD/SR/001
3. Paste Kettle 100 Liter PD/PK/001
4. Rapid Mixer Granulator (RMG) 250 Liter PD/RM/001
Fluidized Bed Dryer (FBD)
5. with product (active ingredient) 120 kg PD/FB/001
specific bag
6. Multimill (1.5 mm, SS ) 100 Kg/ Hrs PD/ML/001
7. Octagonal Blender 1200 Liter PD/OB/001
27 Station Double Rotary Tablet
8. Compression machine with 62500 Tab/Hrs PD/CM/003
necessary accessories
9. Alu-Alu Packing Machine NA PD/BP/001

4.0 PROCESS VALIDATION STRATEGY

Number of batches for process validation
Three Consecutive batches of product will be taken with similar batch size for process validation.
Sr. No. Batch No. Batch Mfg. Date Exp. Date Date of Manufacturing
Size
1.
2.
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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 7 of 18

3.

5.0 APPROVED RAW AND PRIMARY PACKING MATERIALS

The Raw and Packing material used during the manufacturing process are from approved vendors
and are tested for their compliance to ensure that materials are of the acceptable quality prior to
their use.
5.1 RAW MATERIALS
Sr.No. Material Name Approved Vendor
Date: Date: Date:
B.No. B.No. B.No.
1. MCC Plain
2. D.C.P
3. Maize Starch
4. Maize Starch
5. PVPK-30
6. Purified Water
7. Levocetirizine
8. MCC-102 (DC Grade)
9. Crosspovidone XL-10
10. Crosscarmellose
Sodium
11. Sodium Lauryal
Sulphate
12. Colloidal Silicon
Dioxide
13. Talcum
14. Magnesium Stearate
15. M.C.C -102(Excess)
5.2 PRIMARY PACKING MATERIALS
Approved vendor
Material name Date: Date: Date:

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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 8 of 18

B.No. B.No. B.No.

Printed foil
PVC
6.0 MANUFACTURING PROCESS: Check the Machine/Equipment’s to be used during
manufacturing process for cleanliness and status label displayed. Take the line clearance from
IPQA for Area Cleanliness. Record the Temperature NMT 25±2°C and Relative humidity NMT
55± 5 %) of the Manufacturing Room.
6.1 SIFTING:
Check the integrity and cleanliness of sieves Before sifting process.
Integrity Check
Sr. Cleanliness
Sieve(#) Size Before Sifting (Satis. / Not
No. Check (Cleaned/ Not Cleaned)
Satisfactory
Date: Batch No.:-
1. #40
2. #80
Date: Batch No.:-
1. #40
2. #80
Date: Batch No.:-
1. #40
2. #80
Sift the material through 30 #,40 (mesh)

Particulars Observations
Date: Date: Date:
Sieve size80 #,#40, (mesh) B.No. B.No. B.No.

Levocetirizine
MCC Plain
D.C.P
Maize Starch
MCC-102 (DC Grade)
Crosspovidone XL-10
Crosscarmellose Sodium
Sodium Lauryal Sulphate
Colloidal Silicon Dioxide
Talcum
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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 9 of 18

Magnesium Stearate
M.C.C -102(Excess)

Check the integrity and cleanliness of sieves After sifting process.

Sr. Integrity Check Cleanliness
Sieve(#) Size
No. After Sifting (Satis. / Not Satisfactory Check (Cleaned/ Not Cleaned)
Date: Batch No.
1. #40
2. #80
Date: Batch No.
1. #40
2. #80
Date: Batch No.
1. #40
2. #80

6.2 CONCLUSION:
After sifting from .................. found to be within the acceptable limits hence it is concluded that
………...…. is the validated sieve for sifting

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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
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6.3 LUBRICATION:-
During this stage granules are mixed with a lubricant, which is influencing the flow pattern and
content uniformity of the blend for compression of Tablets.
Shift the Lubrication material and add to the blender
Lubrication:
Date(....................) Batch No. :-(....................................)
Material Name Levocetirizine Flow Property
(Assay)%
RT
CT
LT
FT
BT
After 15 Minutes RM
LM
CM
LB
RB
Comp.
RT
CT
LT
FT
BT
After 30 Minutes RM
LM
CM
LB
RB
Comp.
After 60 Minutes RT
CT
LT

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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 11 of 18

FT
BT
RM
LM
CM
LB
RB
Comp.

Date: (........................) Batch No. (..................................)

Material Name Levocetirizine Flow Property
(Assay)%
RT
CT
LT
FT
BT
After 15 Minutes RM
LM
CM
LB
RB
Comp.
RT
CT
LT
FT
BT
After 30 Minutes RM
LM
CM
LB
RB
Comp.
After 60 Minutes RT
CT
LT
FT
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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 12 of 18

BT
RM
LM
CM
LB
RB
Comp.
Date :(......................) Batch No. :-(...............................)
Material Name Levocetirizine Aceclofenac
(Assay)% (Assay %)
RT
CT
LT
FT
BT
After 15 Minutes RM
LM
CM
LB
RB
Comp.
RT
CT
LT
FT
BT
After 30 Minutes RM
LM
CM
LB
RB
Comp.
After 60 Minutes RT
CT
LT
FT
BT
RM
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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
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LM
CM
LB
RB
Comp.

VISUAL INSPECTION: Visual inspection helps to remove the physical defects of the tablets,
thus ensure appearance quality of tablets.
Take the line clearance from IPQA for Area and machines/equipment’s cleanliness and for
unwanted materials. Record the Temperature NMT 25±2 °C and Relative humidity NMT 55 ± 5
% of the Inspection Area
Sr. No. Physical Defects/Rejections
1. Appearance 5. Erosion
2. Picking and Sticking 6. Bridging
3. Capping 7. Cracking
4. Chipping
Load the tablets in the visual inspection table and observe the tablets for the defects and remove
the defects.
PACKING:

Blister Packing Machine:

Date: (....................) Batch No.:- (................................)

Run the machine at different speed and the Different Forming & Sealing temperature.

M/C Speed Temperature Temperatu Leak Test Pocket Printing Appearance

(0C) re (0C) Form Quality
20 Forming Temp Sealing
120 Temp 150
20 Forming Temp Sealing
130 170
20 Forming Temp Sealing
150 210
30 Forming Temp Sealing
120 Temp 150
30 Forming Temp Sealing

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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 14 of 18

130 170
30 Forming Temp Sealing
150 210
40 Forming Temp Sealing
120 Temp 150
40 Forming Temp Sealing
130 170
40 Forming Temp Sealing
150 210
Physical Verification, at Minimum Speed and Maximum Sealing Temperature.

Date: (...................) Batch No.:- (............................)

Run the machine at different speed and the Different Forming & Sealing temperature.

M/C Speed Temperature Temperatu Leak Test Pocket Printing Appearance

(0C) re (0C) Form Quality
20 Forming Temp Sealing
120 Temp 150
20 Forming Temp Sealing
130 170
20 Forming Temp Sealing
150 210
30 Forming Temp Sealing
120 Temp 150
30 Forming Temp Sealing
130 170
30 Forming Temp Sealing
150 210
40 Forming Temp Sealing
120 Temp 150
40 Forming Temp Sealing
130 170
40 Forming Temp Sealing
150 210
Physical Verification, at Minimum Speed and Maximum Sealing Temperature.

Date: (.................) Batch No.:- (...............................)

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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 15 of 18

Run the machine at different speed and the Different Forming & Sealing temperature.

M/C Speed Temperature Temperatu Leak Test Pocket Printing Appearance

0 0
( C) re ( C) Form Quality
20 Forming Temp Sealing
120 Temp 150
20 Forming Temp Sealing
130 170
20 Forming Temp Sealing
150 210
30 Forming Temp Sealing
120 Temp 150
30 Forming Temp Sealing
130 170
30 Forming Temp Sealing
150 210
40 Forming Temp Sealing
120 Temp 150
40 Forming Temp Sealing
130 170
40 Forming Temp Sealing
150 210
Physical Verification, at Minimum Speed and Maximum Sealing Temperature.

Final Result of finish product

Sr. Test Specification Batch No.
No.
1. Description An Orange Coloured
elongated biconvex
having central break
line on one side &
another side plain film
coated tablets.
2. Identification To Be comply
3. Average Weight Limit-(610.0 mg ±
5.0%
4. Uniformity Of weight Avg. Wt ± 5.0%
5. Length Limit-15.00 mm ±
0.02% mm
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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
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6. Width Limit-8.20 mm ±
0.02% mm
7. Thickness Limit-5.50 mm ±
0.02% mm
8. Hardness NLT-4.0kg/cm2
9. Friability NMT-1.0%ww
10. Disintegration Time NMT-15.0Minutes
11. Assay: each film coated tablet Limit-90.00 mg to
contains- 110.0 mg
Aceclofenac 100 mg (NLT-90.0% & NMT-
110.0%)

Paracetamol 325 mg Limit-292.5 mg to

357.5 mg
(NLT-90.0% & NMT-
110.0%)

RESULTS EVALUATION:-
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DEVIATION:-

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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 17 of 18

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STABILITY:-

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ABBREVIATIONS:-

Quality Control Q.C. Flurized Bed Dryer FBD

Quality Assurance Q.A. Raw Material R.M.
Current Good Manufacturing cGMP Rapid Mixing Granulator RMG
practices
Quantity Sufficient q.s. Loss on Drying LOD
Quantity Qty. Finished Goods F.G.
British Pharmacopeia BP Expiry Exp.
Not More Than NMT Air Handling Unit AHU
Manufacturing Mfg. Milligram mg
In Process Quality Assurance IPQA Gram gm
REPORT APPROVAL SHEET:

REPORT PREPARED BY:

NAME DESIGNATION SIGNATURE DATE

REPORT REVIEWED BY:

NAME DESIGNATION SIGNATURE DATE

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 GMH LABORATORIES
Plot No.-13, Industrial Township, Bhatoli Kalan , Baddi Distt.-Solan
(H.P.) 173205

PROCESS VALIDATION REPORT

REPORT No.:
Effective Date:
GMH/PVR/L05/23/01
Levocetirizine Tablets IP
Revision No.: 01 Review Date:
Supersedes: 00 Page No. : 18 of 18

REPORT APPROVED BY:

NAME DESIGNATION SIGNATURE DATE

END OF THE DOCUMENT

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