WINTHROX LABORATORIES PVT.

LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Signatures & Approvals

Prepared by : Miss YumnaFarooq Signature : _________________

(Validation Officer)

Miss Aisha Rehman

Checked by : Signature : _________________
(Compliance Officer)

Miss MeharJabeen
Checked by : Signature : _________________
(Asst. Manager Microbiology)

Miss SehrishKanwal
Reviewed by : Signature : _________________
(Manager Quality Control)

Mr. MazharMasood
Reviewed by : Signature : _________________
( Manager Production)

Miss ShahnazMukhtar
Approved by : Signature : _________________
(Manager Quality Assurance)

Page 1 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

S. NO. TABLE OF CONTENT PAGE NO

01 Approval Page 01
02 Table of content 02
03 List of SOPs 03
04 Objective 04
05 Scope 04
06 Responsibilities 04
Process Validation Phase (I) Process Design
07 List Of Equipment 05
08 List of Instruments 06
09 Process Flow chart 07
10 Risk Assessment 08
11 Product Composition 09
12 List of Packing Material 10
13 Critical Process Parameter 11
Master Test Sheet (Before Manufacturing)
a) Washing of vials
14 12-15
b)Depyrogenation of Glass vials
c)Sterilization of Rubber Stopper
Master Test Sheet (Manufacturing Process)
15 a)Assay of Bulk 16-17
b)Sterility and BET Test of Bulk
Master Test Sheet (Filling Process)
a)Inprocess (Weight variation/Nitrogen purging/Visual Inspection)
16 18-23
b)Assay of Finished Product
b)Sterility and BET Test of Finished Product
17 Critical Quality Attributes 24
18 Packing Stage (Labeling) 25
19 Packing Stage (Blistering) 26
20 Deviation Report 27
21 Report Statement 28

Page 2 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

SOPS FOLLOW IN PROCESS VALIDATION OF

CEFOWIN 1000mg DRY POWDER INJECTION

S. No. Standard Operating Procedure SOP #

SOP for Process Validation

01 QA/PRV/006

02 SOP for Sterility Test for Bulk/ Finished Product MB/SOP/010

03 SOP for Bacterial Endotoxin MB/SOP/011

04 SOP for Cefotaxime Testing AMRM-022

SOP for Testing Method of Cefowin 1000mg Dry Powder

05 AMFP-I010
Injection

06 SOP For of Inprocess of Dry Powder Injection QA/PPS/035

07 SOP for Dispensing WH/SOP/008

08 SOP for Water Testing MB/SOP/015

09 Operating Procedure of Vial Washing Machine PD/STL/WM/003

10 Operating Procedure For Autoclave PD/STL/ACV/004

11 Operating Procedure For Dry Heat Sterilization PD/STL/DHS/005

12 SOP For of Filling of Dry Powder Injection PD/STL/PPF/015

13 Operating procedure of Capping and Sealing Machine PD/STL/PPS/016

Page 3 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

1.0 PROCESS VALIDATION OBJECTIVE:

1.1 Process Validation is carried out to establish documented evidence, which provides high
degree of assurance that manufacturing of Product is consistently produce product with all
quality attributes.
1.2 The validation is based on the evaluation of the in-process controls and physical o-
chemical results pertaining to the critical steps of the manufacturing process.
1.3 Process Validation is carried out to gain ongoing assurance to show that the process
remains in a state of control.

 Validation Approach:
Concurrent Validation

 Validation Strategy:
Validation will be performed on three batches of Cefowin 1000mg Dry Powder Injection.
All critical process parameter related to manufacturing will be evaluated during study. For
critical Quality Attributes of product, analytical data will be compiled from all stages of
manufacturing.

2.0 SCOPE:

This report applies to the Cefowin 1000mg Dry Powder Injection manufactured at Winthrox
Laboratories (Pvt.) Limited and the scope of Process validation linked to quality risk management
(QRM) and quality by design principles.

3.0 RESPONSIBILITIES:

Responsibilities Assign To Team

S. No. Team Members Designation
Members
1 PREPARATION OF VALIDATION Miss Yumna Farooq Validation Officer
PROTOCOL & REPORT
2 PRODUCTION OF VALIDATION Mr. Mazhar Masood Manager Production
BATCHES
3 ANALYSIS OF VALIDATION BATCHES Miss Aisha Rehman Compliance Officer
AND PREPARATION OF REPORTS
4 MICROBIOLOGICAL ANALYSIS Miss Meher Jabeen Microbiologist

REVIEW AND APPROVAL OF Miss Shahnaz Manager Quality

5
VALIDATION PROTOCOL& REPORT Mukhtar Assurance

EQUIPMENT AND MACHINE Maintenance

6 Mr. Faisal
MAINTENANCE Incharge

Page 4 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

PROCESS VALIDATION PHASE-I

1.0 BATCHES TO BE STUDIED:

The process can be considered validated if the first three batches of product satisfy specifications

BATCH MANUFACTURING MANUFACTURING

S. NO. BATCH SIZE
NUMBER AREA DATE
Cephalosporin sterile
01 007CV 9000 05-04-2019
manufacturing area
Cephalosporin sterile
02 036CV 9000 02-11-2019
manufacturing area

Cephalosporin sterile
03 044CV 9000 24-11-2019
manufacturing area

2.0 LIST OF EQUIPMENTS/MACHINES:

EQUIPMENT TO BE QUALIFICATION
S. NO FUNCTIONS ID
USED STATUS

01 Vial Washing Machine Blending PRD/STP-PFM-01 Done

Autoclave For Rubber Filling of Done
02 PRD/STP-AUT-04
stopper(20mm) Powder
Dry Heat Sterilizer for glass Done
03 Sealing PRD/STP-DHS-07
vials(10ml)
Vial Filling & Plugging PRD/STP-PFM-01 Done
04 Filling
Machine
05 Vial Sealing Machine Sealing PRD/STP-PFM-01 Done

Note: Equipment Qualification of all above equipments can be seen recorded in the Equipment
Qualification documents.

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Page 5 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Date: _________________ Date: _________________

Production Incharge Validation Officer

QUALIFICATIO CALIBRATIO
EQUIPMENT DESCRIPTION RESULT
N STATUS N STATUS
TYPE Reverse Phase
CAPACITY 0.1-10 ml/min
HPLC Done Calibrated
MANUFACTURE
SHIMADZU
R
TYPE Precision
WEIGHING RANGE 0.1 mg- 210 g Done Calibrated
BALANCE MANUFACTURE OHAUS
R (Pioneer)
TYPE Pyrex
GLASSWARE Done Calibrated
MANUFACTURE Friends
S
R Engineering
TYPE LOD
KARL CAPACITY (0-15.0%) Done Calibrated
FISCHER MANUFACTURE
OHAUS
R
H1 2210 pH
TYPE
meter Done Calibrated
pH METER
MANUFACTURE HANNA
R Instruments
Mesophillic MANUFACTURE Done Calibrated
Memmert
Incubator R
Psychrophillic MANUFACTURE Done Calibrated
Memmert
Incubator R
Bio Safety MANUFACTURE Done Calibrated
Curio-2020
Cabinet R
3.0 LIST OF INSTRUMENTS:

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Date: _________________ Date: _________________

Page 6 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Quality Control Manager Validation Officer

4.0 PROCESS DESCRIPTION/FLOW CHART:

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Page 7 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Date: _________________ Date: _________________

Quality Control Manager Quality Assurance Manager

5.0 RISK ASSESSMENT:

A risk-based approach to process validation provides a rational framework for developing an

appropriate scope for validation activities, focusing on processes that have the greatest potential risk
to product quality.

S. NO. VALIDATION STAGE CHECKED BY REMARKS

BEFORE FILLING:
1 De-Ionized water should be passed by QC
2 Use masks and gloves during washing
During ampoule washing, observe dust, fiber and
3
foreign particles in the vials.
Autoclave should be qualified and have even
4
temperature distribution
After depyrogenation, vial should be filled with in
5
24 hours
6 Depyrogenate the vial for 1 hour at 250 oC
IN FILLING:
1 SOP for Gowning and Degowning must follow
2 Filling Instructions must be available at location
3 Temperature and Humidity should be controlled
4 Particle Count should be in range
Raw material should be available and placed in
5
the LAF
6 Clean the area as per SOP of Cleaning
7 Particle counter should be calibrated
8 Nitrogen Gas must be from reliable source

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Page 8 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Checked by Verified by

Date: _________________ Date: _________________

Production Incharge Validation Officer

6.0 PRODUCT COMPOSITION:

Raw material used in Filling of Vial should be from approved vendors.

QTY
MATERIAL ITEM QTY KG/ OBSERVATIO APPROVE
S. NO. ROLE mg/
DESCRIPTION CODE BATCH N D VENDOR
VIAL

Nectar life
01 Cefotaxime CFT-129 API 1100 9.9 kg Complies sciences
Ltd.

Note: Certificate of Analysis of above mentioned Active and Excipients should be attached with
the reports as used in the respective BMR.

Approved Vendor List of Active Raw materials should be attached with reports.

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Date: _________________ Date: _________________

Page 9 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Warehouse Officer Validation Officer

7.0 LIST OF PACKAGING MATERIALS:

All the Packaging material used in packing should be from approved vendors.

S. NO. MATERIAL DESCRIPTION APPROVED MANUFACTURER

1 Glass Vials 15ml T.I Pharma

2 Rubber Stoppers T.I Pharma
3 Flip Off (Light blue) United Engineering
4 W.F.I Vial (5ml) Jivani Traders
5 Leaflets Azeem Enterprises
6 Unit Carton Azeem Enterprises

7 Labels Azeem Enterprises

8 Aluminium Foil T.I Pharma

9 PVC Foil T.I Pharma
10 Master Carton Mustafa Packages

Note: Packaging Material (label, unit cartons) must be attached with reports.

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Page 10 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Checked by Verified by

Date: _________________ Date: _________________

Warehouse Officer Validation Officer

Page 11 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

8.0 CRITICAL PROCESS PARAMETER:

Process Parameter Test To Be Carried Out Explanation

Microorganism may produce and area
Temperature By calibrated Hygrometer
will be contaminated

Humidity By calibrated Hygrometer Powder may absorb moisture

By calibrated particle
Environment Control Particles may include in the powder
counter
Filling Process

Weight variation each from Less or more quantity of powder may

start, middle & end of filling affect the quality of product.
Weight Variation
process by calibrated
balance

Sample of eight vials to be

collected for visual test each Particles may cause harm in the
Visual Inspection
from start, middle & end of patient
filling process

Nitrogen Purging
By calibrated nitrogen gas Powder may stick at the wall of vial.

Page 12 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

9.0 MASTER TEST SHEET:

S. No. Before Manufacturing

01 Washing of clear glass vials

02 Depyrogenation of clear glass vials (15ml)

03 Sterilization of Rubber Stopper (20mm)

Manufacturing Process

04 Assay of Raw Material (Cefotaxime )

05 Sterility and BET of bulk sample

Filling Process

06 Weight Variation/Nitrogen purging/Visual inspection

07 Assay of finished product

08 Sterility test /BET of finished product

Page 13 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

9.1 TEST SHEET:

Washing of Glass Vials

A. TEST CONDITION & SAMPLING PLAN:

N/A

B. ACCEPTANCE CRITERIA:
Source of Clear glass vials (15ml): Vials should be from approved source.
QC Testing Status: Result complies with specification limit.

C. DATA:

Batch No DI water Status Visual Inspection Remarks

007CV Passes Complies Satisfactory
036CV Passes Complies Satisfactory
044CV Passes Complies Satisfactory

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Date: _________________ Date: _________________

Microbiologist Validation Officer

Page 14 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

9.2 TEST SHEET:

Depyrogenation of Clear Glass vials

A. TEST CONDITION & SAMPLING PLAN:

For testing, Collect 20 vials after the process of depyrogenation & before the process of
manufacturing

B. ACCEPTANCE CRITERIA:
No Gel formation Found

C. DATA:

Bacterial Endotoxin test Results

Sampling
Batch No: 007CV Batch No: 036CV Batch No: 044CV
Start No gel No gel No gel
Middle No gel No gel No gel
End No gel No gel No gel
Mean No gel No gel No gel

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Date: _________________ Date: _________________

Microbiologist Validation Officer

Page 15 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

9.3 TEST SHEET

Sterilization of Rubber Stopper

A. TEST CONDITION & SAMPLING PLAN:

For testing, collect the rubber stopper from each bag in sterile polybag after the sterilization &
before start the filling (About 20)

B. ACCEPTANCE CRITERIA:
It should be Sterile

C. DATA:

Sterility Test Results

Sampling
Batch No: 007CV Batch No: 036CV Batch No: 044CV
Start Sterile Sterile Sterile
Middle Sterile Sterile Sterile
End Sterile Sterile Sterile
Mean Sterile Sterile Sterile

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Date: _________________ Date: _________________

Microbiologist Validation Officer

Page 16 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

9.4 TEST SHEET:

RAW Material (BULK) Testing (Cefotaxime)

A. TEST CONDITION & SAMPLING PLAN:

For Assay test, 10g sample to be collected from the container under Laminar.

OBSERVATIONS
PROCESS/
SPECIFICATION BATCH NO. BATCH NO. BATCH NO.
TESTS REMARKS
007CV 036CV 044CV

White to off White

Description Complies Complies Complies satisfactory
crystalline Powder

By HPLC
Identification Complies Complies Complies satisfactory
Chromatography

Water Content NMT 3.0% 1.9 2.1 2.3 satisfactory

pH (4.5-6.5) 5.17 5.12 5.24 satisfactory

Assay
Ceftriaxone (91.6-96.4) % ODB 92.85 92.44 93.06 satisfactory
Sodium

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Page 17 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Checked by Verified by

Date: _________________ Date: _________________

Quality Control Manager Validation Officer

9.5 TEST SHEET:

Sterility And Bacterial Endotoxin(Bulk)

A. TEST CONDITION & SAMPLING PLAN:

For Sterility and Bacterial Endotoxin test, collect the sample10g in sterile vial from Container
under Laminar.

RESULTS
COUNT OF
S. NO. SPECIFICATION Batch No: Batch No: Batch No:
ORGANISM
REMARKS
007CV 036CV 044CV

1 Sterility Should be Sterile Sterile Sterile Sterile Satisfactory

Bacterial No gel No gel Satisfactory

2 0.2EU/mg No gel
Endotoxin

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Date: _________________ Date: _________________

Microbiologist Validation Officer

Page 18 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Page 19 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

9.6 TEST SHEET:

Inprocess During Filling of Injection (weight variation/Nitrogen Purging/Visual

Inspection)

A. TEST CONDITION & SAMPLING PLAN:

For weight variation/Nitrogen purging/Visual Inspection, collect the vials from
each plunger at different intervals of Powder Filling:

B. ACCEPTANCE CRITERIA:

Weight Variation: 1100mg/vial ± 2% (1078-1122) mg/vial

Visual Inspection: No particles found during visual inspection.
Nitrogen Purging: No powder observe at wall of vial during nitrogen purging observation

Page 20 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Batch
No. Wt. of Humidit Temperatur Nitrogen Visual
Capping/Sealing
powder y e Purging Inspection
1083mg 30% 25ºC Satisfactory ok Complies
1080 mg 33% 25 ºC Satisfactory Ok Complies
1079 mg 31% 24 ºC Satisfactory Ok Complies
1090 mg 35% 25 ºC Satisfactory Ok Complies
1089 mg 33% 24 ºC Satisfactory Ok Complies
1101 mg 34% 23 ºC Satisfactory Ok Complies
1112 mg 31% 24 ºC Satisfactory Ok Complies
1096 mg 30% 25 ºC Satisfactory Ok Complies
1084 mg 34% 24 ºC Satisfactory Ok Complies
1085 mg 35% 25 ºC Satisfactory Ok Complies
1092 mg 33% 24 ºC Satisfactory Ok Complies
1100 mg 34% 25 ºC Satisfactory Ok Complies
007CV 1095 mg 30% 24 ºC Satisfactory Ok Complies
1080 mg 33% 24 ºC Satisfactory Ok Complies
1086 mg 31% 23 ºC Satisfactory Ok Complies
1010 mg 35% 24 ºC Satisfactory Ok Complies
1089 mg 33% 25 ºC Satisfactory Ok Complies
1088 mg 34% 24 ºC Satisfactory Ok Complies
1092 mg 31% 24 ºC Satisfactory Ok Complies
1091 mg 33% 23 ºC Satisfactory Ok Complies
1079 mg 31% 24 ºC Satisfactory Ok Complies
1010 mg 33% 24 ºC Satisfactory Ok Complies
1112 mg 33% 24 ºC Satisfactory Ok Complies
1086 mg 34% 23 ºC Satisfactory Ok Complies
1093 mg 35% 24 ºC Satisfactory Ok Complies

Batch
No. Wt. of Humidit Temperatur Nitrogen Visual
Capping/Sealing
powder y e Purging Inspection

Page 21 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

1081mg 31% 24 ºC Satisfactory ok Complies

1085 mg 30% 25 ºC Satisfactory Ok Complies
1089 mg 33% 24 ºC Satisfactory Ok Complies
10800
35% 25 ºC Satisfactory Ok Complies
mg
1092 mg 33% 24 ºC Satisfactory Ok Complies
1105 mg 33% 23 ºC Satisfactory Ok Complies
1104 mg 34% 24 ºC Satisfactory Ok Complies
1086 mg 35% 25 ºC Satisfactory Ok Complies
1092 mg 33% 24 ºC Satisfactory Ok Complies
1095 mg 34% 24 ºC Satisfactory Ok Complies
1092 mg 31% 25 ºC Satisfactory Ok Complies
1101 mg 30% 25 ºC Satisfactory Ok Complies
036CV
1085 mg 33% 24 ºC Satisfactory Ok Complies
1091 mg 35% 23 ºC Satisfactory Ok Complies
1096 mg 33% 24 ºC Satisfactory Ok Complies
1104 mg 33% 25 ºC Satisfactory Ok Complies
1079 mg 34% 24 ºC Satisfactory Ok Complies
1090 mg 35% 24 ºC Satisfactory Ok Complies
1095 mg 33% 24 ºC Satisfactory Ok Complies
1092 mg 34% 23 ºC Satisfactory Ok Complies
1105 mg 31% 24 ºC Satisfactory Ok Complies
1104 mg 30% 24 ºC Satisfactory Ok Complies
1086 mg 34% 24 ºC Satisfactory Ok Complies
1092 mg 35% 23 ºC Satisfactory Ok Complies
1095 mg 33% 24 ºC Satisfactory Ok Complies

Batch
No. Wt. of Humidit Temperatur Capping/Sealin Nitrogen Visual
powder y e g Purging Inspection
044CV 1086 mg 31% 24 ºC Satisfactory ok Complies
1092 mg 30% 25 ºC Satisfactory Ok Complies

Page 22 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

1095 mg 33% 24 ºC Satisfactory Ok Complies

1092 mg 31% 23 ºC Satisfactory Ok Complies
1101 mg 33% 24 ºC Satisfactory Ok Complies
1085 mg 33% 25 ºC Satisfactory Ok Complies
1091 mg 34% 24 ºC Satisfactory Ok Complies
1096 mg 35% 23 ºC Satisfactory Ok Complies
1104 mg 33% 24 ºC Satisfactory Ok Complies
1079 mg 34% 25 ºC Satisfactory Ok Complies
1090 mg 31% 24 ºC Satisfactory Ok Complies
1089 mg 30% 24 ºC Satisfactory Ok Complies
1101 mg 33% 24 ºC Satisfactory Ok Complies
1112 mg 31% 23 ºC Satisfactory Ok Complies
1096 mg 33% 24 ºC Satisfactory Ok Complies
1084 mg 33% 25 ºC Satisfactory Ok Complies
1085 mg 34% 24 ºC Satisfactory Ok Complies
1092 mg 35% 24 ºC Satisfactory Ok Complies
1100 mg 33% 24 ºC Satisfactory Ok Complies
1095 mg 33% 23 ºC Satisfactory Ok Complies
1085 mg 33% 24 ºC Satisfactory Ok Complies
1091 mg 33% 24 ºC Satisfactory Ok Complies
1096 mg 34% 24 ºC Satisfactory Ok Complies
1104 mg 35% 23 ºC Satisfactory Ok Complies
1079 mg 33% 24 ºC Satisfactory Ok Complies

If any deviation is observed. Note down in the deviation report, located at the back of this document.
Remarks

Checked by Verified by
Date: _________________ Date: _________________

Production Incharge Validation Officer

9.7 TEST SHEET:

Analytical Testing of Finished Product

A. TEST CONDITION & SAMPLING PLAN:

For Assay test, 10 vials to be collected at start, middle & end of filling.

Page 23 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

PROCESS OBSERVATIONS
SPECIFICATI
/ Batch No Batch No Batch No REMAR
ON
TESTS 007CV 036CV 044CV KS
White to Off
White
complies

complies

complies

complies

complies

complies
complies

complies

complies
Crystalline satisfactor
Description
Powder after y
reconstitution
produce
complies

complies

complies

complies

complies

complies
complies

complies

complies
1)By HPLC satisfactor
Identificati
on Chromatography y

satisfactor
pH (4.5-6.5) 5.19 5.11 5.15 5.05 5.07 5.02 5.25 5.25 5.22 y

(90.00-115.00) satisfactor
Assay 99.9 100.0 99.9 100.1 100.0 99.7 99.9 99.8 99.9
Cefotaxime % 4 1 5 1 5 5 8 9 4 y

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Date: _________________ Date: _________________

Quality Control Manager Validation Officer

9.8 TEST SHEET:

Sterility And Bacterial Endotoxin (Bulk)

Page 24 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

A.TEST CONDITION & SAMPLING PLAN:

For Sterility testing and Bacterial Endotoxin test collect 20vials at start, middle & end of filling.

RESULTS
COUNT OF SPECIFICATIO
S. NO. Batch No Batch No Batch No REMARK
ORGANISM N
007CV 036CV 044CV S

Sterile Sterile Sterile satisfactor

1 Sterility Should be Sterile
y

Complies Complie
2 Bacterial Endotoxin 0.2EU/mg Complies satisfactory
s

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Date: _________________ Date: _________________

Microbiologist Validation Officer

10.0 CRITICAL QUALITY ATTRIBUTES:

Page 25 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

TEST TO BE CARRIED
S. NO. QUALITY EXPLANATION
OUT
ATTRIBUTES

To meet label claim (Less or

It should be done by more quantity may effects
1 Assay
Calibrated HPLC strength of the products and
also effects the patients

Bacterial Endotoxin Pyrogen may produce which

2 By BET kit
Test cause fever

Microorganism contamination
3 Sterility Test By TFM and TSM
may cause harm to patient

11.0 PACKING STAGE:

Page 26 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Labeling:

During labeling of Cefowin 1000mg dry powder injection, QA will inspect the labeling process:

BATCH NO: 007CV

No of
Alignment Label Pasting B.No/Mfg/Exp/MRP Label Claim
Vials
01 OK OK 007CV/04.19/04.21/195.73 OK
02 OK OK 007CV/04.19/04.21/195.73 OK
03 OK OK 007CV/04.19/04.21/195.73 OK
04 OK OK 007CV/04.19/04.21/195.73 OK
05 OK OK 007CV/04.19/04.21/195.73 OK
BATCH NO: 036CV
01 OK OK 036CV/11.19/11.21/195.73 OK
02 OK OK 036CV/11.19/11.21/195.73 OK
03 OK OK 036CV/11.19/11.21/195.73 OK
04 OK OK 036CV/11.19/11.21/195.73 OK
05 OK OK 036CV/11.19/11.21/195.73 OK
BATCH NO: 044CV
01 OK OK 044CV/11.19/11.21/195.73 OK
02 OK OK 044CV/11.19/11.21/195.73 OK
03 OK OK 044CV/11.19/11.21/195.73 OK
04 OK OK 044CV/11.19/11.21/195.73 OK
05 OK OK 044CV/11.19/11.21/195.73 OK

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Date: _________________ Date: _________________

Production Incharge Validation Officer

Page 27 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Blistering:

During blistering of Cefowin 1000mg dry powder injection, QA will inspect the blistering process:

BATCH NO: 007CV

No of Physical Inspection
Cutting Sealing
Vials Vial (B. No/Mfg/Exp date) WFI (B. No/Mfg/Exp date)
01 007CV/04.19/04.21 399/11.18/10.21 OK OK
02 007CV/04.19/04.21 399/11.18/10.21 OK OK
03 007CV/04.19/04.21 399/11.18/10.21 OK OK
04 007CV/04.19/04.21 399/11.18/10.21 OK OK
05 007CV/04.19/04.21 399/11.18/10.21 OK OK

BATCH NO: 036CV

01 036CV/11.19/11.21 007A/11.19/11.21 OK OK
02 036CV/11.19/11.21 007A/11.19/11.21 OK OK
03 036CV/11.19/11.21 007A/11.19/11.21 OK OK
04 036CV/11.19/11.21 007A/11.19/11.21 OK OK
05 036CV/11.19/11.21 007A/11.19/11.21 OK OK

BATCH NO: 044CV

01 044CV/11.19/11.21 007A/11.19/11.21 OK OK
02 044CV/11.19/11.21 007A/11.19/11.21 OK OK
03 044CV/11.19/11.21 007A/11.19/11.21 OK OK
04 044CV/11.19/11.21 007A/11.19/11.21 OK OK
05 044CV/11.19/11.21 007A/11.19/11.21 OK OK

If any deviation is observed. Note down in the deviation report, located at the back of this document.

Remarks

Checked by Verified by

Date: _________________ Date: _________________

Production Incharge Validation Officer

Page 28 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

DEVIATION REPORT

The following is a description of the deviations, which were observed during study. Use additional
pages as necessary.

Reference (Test # &Page#)

Discrepancy/Variation

Resolution

Acceptable Yes No

Signature Date

Page 29 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

REPORT STATEMENT

The validation is based on the evaluation of the in-process controls and physico-chemical results
pertaining to the critical steps of the Manufacturing Process.

__________________________________________________________________________________
__________________________________________________________________________________
__________________________________________________________________________________
_______________________________________________________________________________

Comments (if any)

___________________________________________________________________________________
___________________________________________________________________________________
___________________________________________________________________________________

Name: ___________________

Sign/Date_________________

Final Statement

____________________________________________________________________________________
____________________________________________________________________________________
____________________________________________________________________________________

Name ___________________

Page 30 of 31
 WINTHROX LABORATORIES PVT. LTD
QUALITY ASSURANCE DEPARTMENT

Title: Process Validation Report Department Document No.

Subject: Cefowin 1000mg Dry Powder Quality Assurance
QA/PV/PPS/006
Injection
Effective Date Revision Supersede
19-03-2020 00 New Document

Sign/Date _________________

Page 31 of 31