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Company Name and Address VALIDATION

PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 1 of 26

Process Validation
Protocol For
XXXXXXXXXX

Company Name and Address

1. Table of Contents

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Company Name and Address VALIDATION
PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 2 of 26
1. Table of Contents.........................................................................................................................................2

2. Signatories...................................................................................................................................................3

3. Revision status:............................................................................................................................................4

4. Aim..............................................................................................................................................................5

5. Purpose........................................................................................................................................................5

6. Scope...........................................................................................................................................................5

7. Responsibility..............................................................................................................................................5

8. Manufacturing conditions............................................................................................................................6

9. Process Equipment’s....................................................................................................................................7

10. Raw Materials and Packing Materials...................................................................................................11

11. Validation Plan.......................................................................................................................................15

12. Critical Process Controls, sampling plan and acceptance criteria:........................................................21

13. Packaging and storage:..........................................................................................................................24

14. Validation Acceptance Criteria:.............................................................................................................24

15. Changes and deviations:........................................................................................................................25

16. Validation summary:..............................................................................................................................26

17. References:............................................................................................................................................26

18. Annexure:..............................................................................................................................................26

2. Signatories
This document contains 25 pages and is prepared, reviewed and approved by following persons:

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Company Name and Address VALIDATION
PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 3 of 26
Prepared By:
Designation Signature Date
Mr. XXXXXXXXX

Sr. Executive-PR
Reviewed By:
Designation Signature Date
Mr. XXXXXXXX

Sr. Manager - PR
Designation Signature Date
Mr. XXXXXXXXXXX

Dy. Manager - PD

Designation Signature Date

Mr. XXXXXXXXX

Asst. Manager - QC

Designation Signature Date

Mr. XXXXXXXXX

Manager- EG

Designation Signature Date

Mr. XXXXXXXXXX

Executive - QA
Approved By:
Designation Signature Date
Mr. XXXXXXX

Asst. Manager - QA

3. Revision status:

Sr. No. Date Revision Changes Made

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Company Logo PROCESS
Company Name and Address VALIDATION
PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 4 of 26

1 13/06/2019 R00 Initial copy

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Company Name and Address VALIDATION
PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 5 of 26
4. Aim
The aim of this validation protocol is to provide the validation of (Product Name) manufacturing
process as per in line with BMR No. XXXXXXXXXX.
5. Purpose
To conduct the process validation of the manufacturing process for the (Product Name) manufactured at
the Plant-II and Plant-III The validation study shall be conducted for the generation of sufficient data to
establish documentary evidence and to provide assurance that the product can be manufactured with
established parameter on a commercial scale meeting all its quality attributes in a consistent manner.

6. Scope
This protocol shall be applicable for three consecutive commercial scale up batches manufactured with
BMR XXXXXXXXXX with specific batch size, equipment & operating parameter for the process.

7. Responsibility
Functional responsibility is with the validation team comprising of:
 Quality Assurance Shall be responsible for :
1. Approval & training of validation protocol, review of the data compiled, review of deviation (if
any), monitoring of the process as per process parameter & monitoring of withdrawal of validation
sample.
2. Review of the facility, equipment qualification & utility validation report.
3. cGMP compliance during the manufacturing process review & evaluation of data /Result generated
during validation process.
4. Preparation of process validation summary report, review & its approval.
 Production Shall be responsible for :
1. To execute the batches as per BMR & process validation protocol.
2. Preparation of process validation protocol with the help of QA.
3. Compilation of data related to manufacturing area and furnish the same for review.
4. Review of protocol and summary report.
 Quality Control Shall be responsible for :
1. Raw material and packing material analysis.
2. Inprocess and finished product sampling and analysis as per sampling plan.
3. Collection and review of Inprocess and finished product analysis data.
4. Submission of data / Result to QA & production for review & evaluation.

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Company Name and Address VALIDATION
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Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 6 of 26
 Process Development Shall be responsible for:
1. To monitor activities related to execution of the process validation in coordination with Production
and QA.
 Engineering Shall be responsible for:
1. To review the protocol and provide support with equipment’s, facility and manufacturing
condition.

8. Manufacturing conditions:
Temperature of the manufacturing area is not critical and manufacturing shall be carried out at ambient
temperature& for process operations from filtration to packing in ISO Class 8 area.

8.1 Product Details:

1.
Product name (Product Name)
2.
Generic name (Product Name)

3.
Chemical name XXXXXXXXXXXX

4.
Shelf life 5 years

5.
Storage condition XXXXXXXXXXXXXXX.

6.
Batch size XXXXXX kg
7.
Packing instruction Packing style
8.
Use XXXXXXXX

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Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 7 of 26

9. Process Equipment’s
Qualification
Status & Capacity/
Sr. Equipment Equipment Details of Control and
Preventive MOC/RPM Purpose
No. Name Code Measuring Equipment
Maintenance etc.
( Due Date)

Working
Capacity
Qualification VG-R-211/01
2000 L
Due Date: Range 760 mm Hg – 0
XXXXXX MOC Sodium
XXXXXXX SSR TI-R-211/01 hydroxide
1. SS Reactor Range 0 to 400⁰C
Preventive solution
RPM preparation
maintenance TS-R-211/01
50
Due Date: Range 0 to 200⁰C
XXXXXXX Agitator
Anchor

PG-R-212/01
Range 0 to 7 Kg/cm2
Working PG-R-212/02
Qualification Capacity Range 0 to 10.6 Kg/cm2
Due Date: 3000 L PG-R-212/03
20 Oct 2020 Range 0 to 4 Kg/cm2
Glass Lined MOC
2. R-212 GLR VG-R-212/01 Reaction
Reactor Preventive Range 760 mm Hg – 0
maintenance RPM TS-R-212/01
Due Date: 102 Range 0 to 200°C
16 Aug.2019
Agitator
TI-R-212/01
Impeller
Range 0 to 200°C

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Company Name and Address VALIDATION
PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 8 of 26
Qualification
Status & Capacity/
Sr. Equipment Equipment Details of Control and
Preventive MOC/RPM Purpose
No. Name Code Measuring Equipment
Maintenance etc.
( Due Date)

PG-R-213/01
Working Range 0 to 7 Kg/cm2
Qualification Capacity PG-R-213/02
Due Date: 4000 L Range 0 to 10.6 Kg/cm2
27 Nov 2019 VG-R-213/01
Glass Lined MOC
3. R-213 GLR Range 760 mm Hg – 0 Reaction
Reactor Preventive TS-R-213/01
maintenance RPM Range 0 to 200°C
Due Date: 98
22June2019 TI-R-213/01
Agitator
Range 0 to 200°C
Impeller

Working
Capacity
Qualification VG-R-214/01
6000 L
Due Date: Range 760 mm Hg – 0
06 Dec 2019 MOC
R-214 SSR TI-R-214/01 Water
4. SS Reactor Range 0 to 400⁰C
Preventive Washing
RPM
maintenance TS-R-214/01
60
Due Date: Range 0 to 200⁰C
23 June2019 Agitator
Anchor

Qualification
Due Date:
Capacity
20 Oct 2020
48” Dia. RTM-01
5. Centrifuge CF-202 Isolation
Preventive Range 200 to 2000 LPH
MOC
maintenance
SS
Due Date:
22June2019

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Company Name and Address VALIDATION
PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 9 of 26
Qualification
Status & Capacity/
Sr. Equipment Equipment Details of Control and
Preventive MOC/RPM Purpose
No. Name Code Measuring Equipment
Maintenance etc.
( Due Date)
Qualification
Due Date:
Capacity
20 Oct 2020
48” Dia. RTM-01
6. Centrifuge CF-203 Isolation
Preventive Range 200 to 2000 LPH
MOC
maintenance
SS
Due Date:
23Aug 2019

Qualification
PG-TD-303/01
Due Date:
Capacity Range 0 to 7 Kg/cm2
24 Jan 2020
96 Trays TS-TD-303/01
7. Tray Dryer TD-303 Range 0 to 200⁰C Drying
Preventive
maintenance MOC
SS TI-TD-303/01
Due Date: Range 0 to 200⁰C
20 July2019

Working
Qualification Capacity
Due Date 125 Kg/hrs.
07 March 2021
8. Multimill MM-304 Preventive MOC NA Milling
maintenance SS
Due Date: Mesh Size
16Aug 2019 0.5 mm
Working
Qualification Capacity
Due Date 36”.
20 Dec 2019
9. Sifter SFR-303 Preventive MOC NA Sifting
maintenance SS
Due Date: Mesh Size
17June2019 10 mm

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PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 10 of 26

Details of QC instruments :
Sr. Equipment Equipment
Make Calibration Status Purpose
No. Name ID
Cal. Due date:
1. HPLC M/QC/I/003 AGILENT Analysis
18/08/2019
Cal. Due date:
2. HPLC M/QC/I/004 AGILENT Analysis
15/08/2019
Cal. Due date:
3. HPLC M/QC/I/076 AGILENT Analysis
16/06/2019
Cal. Due date:
4. HPLC M/QC/I/097 SHIMADZU Analysis
30/06/2019
UV
Cal. Due date:
5. Spectrophotom M/QC/I/104 Shimadzu Analysis
18/06/2019
eter
Cal. Due date:
6. GC M/QC/I/013 PERKIN ELMER Analysis
14/06/2019
Cal. Due date:
7. GC M/QC/I/077 AGILENT Analysis
19/06/2019
Cal. Due date:
8. IR M/QC/I/023 SHIMADZU Analysis
09/08/2019
Auto Titrator & Cal. Due date:
9. M/QC/I/107 Metrohm Analysis
KF Titrator 21/08/2019
Cal. Due date:
10. Vacuum oven M/QC/I/017 SHEETAL Analysis
02/12/2019
PATHAK Cal. Due date:
11. Drying oven M/QC/I/016 Analysis
ELECTRICALS 02/12/2019
GALAXY
Cal. Due date:
12. Muffle Furnace M/QC/I/056 SCIENTIFIC Analysis
02/12/2019
EQPT.
Cal. Due date:
13. Muffle furnace M/QC/I/079 NA Analysis
02/12/2019

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Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 11 of 26

10. Raw Materials and Packing Materials

10.1 Raw Material
Sr.
No Code Ingredient Vendor Name Spec No Rationale
.
XXXXXXX Key Raw
1. XXXXXXX XXXXXXX In-house
material
2. - XXXXXXX In-house XXXXXXX Washing
XXXXXXX XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXX XXXXXXX
3. XXXXXXX Solvent
X XXXXXXX
for
XXXXXXX
reaction
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX XXXXXXX
XXXXXXX
4. XXXXXXX XXXXXXX XXXXXXX Reagent
XXXXXXX
XXXXXXX
5. XXXXXXX XXXXXX XXXXXXX XXXXXXX Acid
X XXXXXXX
XXXXXXX
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Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 12 of 26
Sr.
No Code Ingredient Vendor Name Spec No Rationale
.
M/s. Heetu chemicals & alkalies ltd.
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX XXXXXXX
XXXXXXX
XXXXXXX
XXXXXX
6. XXXXXXX XXXXXXX Reagent
X
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX Solvent
XXXXXX
7. XXXXXXX XXXXXXX for
X
XXXXXXX washing
XXXXXXX
XXXXXXX
XXXXXXX

10.2 Packing Materials

Sr.
Code Ingredient Vendor Name Spec No Rationale
No.
XXXXXXX XXXXXXX
XXXXXXX Primary
01 XXXXXXX XXXXXXX
packing
XXXXXXX
XXXXXXX XXXXXXX
XXXXXXX
XXXXXXX
Black XXXXXXX Primary
02 XXXXXXX Polythene bag
XXXXXXX packing
(33” x 66”)
XXXXXXX
XXXXXXX
XXXXXXX XXXXXXX XXXXXXX
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Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 13 of 26
XXXXXXX
HDPE full
XXXXXXX Secondary
03 open top drum
packing
(120 lit.) XXXXXXX
HDPE full XXXXXXX XXXXXXX
Secondary
04 XXXXXXX open top drum
packing
(60 lit.)
Black XXXXXXX XXXXXXX
XXXXXXX Primary
05 XXXXXXX Polythene bags
packing
(50[L]X30[W]) XXXXXXX
Transparent XXXXXXX XXXXXXX
Primary
06 XXXXXXX Polythene bags XXXXXXX
packing
(50[L]X30[W] ) XXXXXXX
Fiber Board XXXXXXX XXXXXXX
Secondary
07 XXXXXXX Drums XXXXXXX
packing
(18X28)
UN No. HDPE XXXXXXX XXXXXXX Secondary
08 XXXXXXX Drum Capacity packing
120 L-SEA
UN No. HDPE XXXXXXX XXXXXXX Secondary
09 XXXXXXX Drum Capacity packing
120 L-AIR
UN No. HDPE XXXXXXX XXXXXXX Secondary
Full Open packing
10 1200001443
Drum CAP –
60 L SEA
UN No. HDPE XXXXXXX Secondary
Full Open packing
11 1200001444 XXXXXXX
Drum CAP –
60 L AIR

Note:
 Raw material and packaging material shall confirm to the In-house specifications.

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Company Name and Address VALIDATION
PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 14 of 26
11. 0 Validation Plan
11.1 Process Details for Manufacturing of (Product Name):
11.1.1 Dissolution of XXXXXXX in XXXXXXX:
Apply vacuum to the reactor R-212 / R-213 and charge XXXX L XXXXX in to reactor. Release the
vacuum of Reactor. Open the manhole Charge XXXX Kg. of XXXX Slowly in Reactor R-212/
R-213 under stirring, after the charging close the manhole properly.
Charge XXXXXX XXXX Kg in Glass Flask GF-208/GF-213 from Tank ST-207 by gravity.
Charge slowly hydrochloric acid XXX Kg at XXXX°C in R-212/R-213 under stirring.
Stir the reaction mass for XX Min. at XXXX°C.
After charging of XXXXXXX clean the Glass Flask GF-208/GF-213 with XXXXXX till
Neutral pH. Check the pH on pH paper.
Withdrawn the sample and check clarity of Reaction mass from reactor. Reaction mass should be
Clear. If Reaction mass is not clear then stir the reaction mass for further XX min at XX °C.
11.1.2 Preparation of XXXXXXXXX Solution:
Take XX L. purified water in cleaned HDPE drum & add XX Kg XXXXXXXXX slowly. Stir with
HDPE/Teflon rod. (XXXXXXXX should not expose with MS, SS item and solvent vapor). Apply
vacuum to the Glass Flask GF-208/GF-213 and charge XXXXXXX solution in Glass flask. Slowly
start addition of XXXXXXX solution in R-212/R-213 under stirring in allow to raise the temp. and
maintain between XXXXX °C in XXX Hrs.
After the complete addition of XXXX solution, maintain reaction mass at XXXX°C.
(if temp below XX°C then apply hot water to the jacket of reactor to achieve temp XXXX°C).
Stir th reaction mass at XXX°C for XX min. Withdraw the sample from reactor R-212/ R-213 for
HPLC test. (To check XXXXXXX content (NMT 1.0 %) & XXXXXXXXXX (NMT 3.5 %).
If HPLC results is not complies add XXXXXXX solution (XXXXXXXXX & water in the
ratio 1:2) as per reaction requirement and continue reaction monitoring up to XXXXXXXX content
within the limit. Cool the reaction mass to XXXXXX C.

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Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 15 of 26
11.1.3 Preparation of XXXXXXXXXXXX Solution in to reactor & pH adjustment:
Charge XXX L. Water in reactor apply chilling to reactor and keep water under stirring Open
manhole and charge XX Kg XXXXXXXXXX slowly under stirring in reactor. Chill solution to XX
– XX C. Transfer the above chilled caustic solution to receiver V-208A/V-213.
Add slowly prepared XXXXXXXX solution at XX –XXC to R-212 / R-213 and adjust the pH
X-X by using Sodium Hydroxide solution. Record the temperature. After complete addition stir the
reaction mixture and cool to XX – XX C and maintain for XX min.

11.1.4 Isolation of the Crude Product by Centrifuge (CF-202 & CF-203):

Apply continuous Nitrogen pressure to the Centrifuge for XX minutes and check oxygen percentage.
(Limit- NMT X %). Open the bottom valve of the R-212/R-213 & feed the material to the Centrifuge
CF-202/CF-203. Collect the mother liquor in centrifuge receiver. Spin dry the wet cake by running
the centrifuge at high speed for XX-XX Min. Switch off the centrifuge and allow to stop completely.
Stop centrifuge for XX-XX min. for Relaxation time. Unload the product (Wet cake) in HDPE drums
lined with new polybag. Transfer the material to Reactor area for slurry.

11.1.5 Preparation of Slurry in Reactor:

Charge XXX L water in reactor R-212/R-213. Open the manhole and charge wet cake in Reactor R-
212/R-213 under stirring, after the charging close the manhole properly. Heat the reaction mixture at
XX-XX°C & Stir for XX min.

11.1.6 Hot Purified water

Charge XXXX L Purified water to Reactor R-214. Heat the purified water up to XX to XX and use
the same hot water for washing in Centrifuge.

11.1.7 Isolation of the Product in Centrifuge & water wash:

Apply continuous Nitrogen pressure to the Centrifuge for XX minutes and check oxygen percentage.
(Limit- NMT X %). Open the bottom valve of the R-212/R-213 & feed the material to the Centrifuge
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Company Name and Address VALIDATION
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Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 16 of 26
CF-202/CF-203. Collect the mother liquor in centrifuge receiver. Drain the ML to ETP. Wash the cake
in centrifuge with hot water from R-214 (XXX L). Wash the cake with Purified water (XX L) from R-
214. Spin the centrifuge till complete removal of washing ML. Drain the ML to ETP.

11.1.8 Washing with Fresh XXXXXXX :

Wash the cake in centrifuge with fresh XXXXX from CFT-203 (90 L). Note the XXXXX ML
Quantity. Spin dry the wet cake by running the centrifuge at high speed for XX-XX Min. switch off
the centrifuge and allow to stop completely. XX-XX min for relaxation then Unload the product
(Wet Cake) in HDPE drums lined with new polybag. Transfer the material to Tray Dryer TD-303for
drying.

11.1.9 Drying of the (Product Name) in Tray Dryer (TD-303):

Open the door of tray dryer and take out the trays. Charge the wet cake in the trays with the help of
SS scoop and place the trays in trolleys. Switch on the fan & allow to air drying for XX-XX Min.
Start heating to the Tray Dryer by opening the steam valve heat to XXX-XXXC. Maintained at
XX-XXC for XXX min. and record the temp details. Cool the product at Room Temperature.
Unload the dried product in HDPE drums lined with polybag.

11.1.10 Milling of (Product Name) (MM-304):

Place the HDPE drums with polybag below the outlet of Multimill for collecting the milled material.
Slowly charge the dried material in to the Multimill charging hopper by SS scoop and switch on the
Multimill. Continue the milling operation till batch quantity completes. Check the integrity of mesh
visually after completion of milling. Integrity: Satisfactory / Not Satisfactory.
11.1.11 In process Sample: Send the In process Sample intimation note given to QC for composite sample
of milled (Product Name) for Description, color value &pH.

11.1.12 Sifting (SFR-303):

Place the HDPE/Fibre board drum lined with poly bag below the outlet nozzle of sifter for collecting
the sifted material. Switch ON the Sifter and slowly charge the material in to the Sifter by SS scoop.
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Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 17 of 26
Continue the sifting operation till batch quantity complete. Check the integrity of sieve visually after
completion of sieving. Integrity: Satisfactory / Not Satisfactory.

Note:
If the integrity is not satisfactory, replace it with a new one and sieve the entire batch quantity again.
11.1.13 Packaging:

Product shall be packed in transparent Polythene bag Qty. Qs then placed in Black Polythene bag
Qty. Qs and then placed in HDPE/Fiber Board Container.

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Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
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Process Flow

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Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
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11.2 Batch details:

Batch operation shall be carried out as per approved Batch Manufacturing record. Three consecutive
batches shall be taken for validation studies. Batch number, Batch size in kg. Shall be recorded in
validation report.

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Documents No. XXXXXXxXX
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12. Critical Process Controls, sampling plan and acceptance criteria:

Method Of Sampling

Quantity of sample

Acceptance criteria
BMR Step No.

Responsibility
Parameter

Frequency

Remarks
Process

During
Temperature
Addition of Every 60 Production

CPP
1.2 and NA NA 30-45°C
XXXXXX min
Time
Solution
Stir reaction Temp. 45-
Temperature
mass at 45- 50ºC and

CPP
2.5 and NA NA -- Production
50ºC for 60 Time 60
Time
min. min.
XXXXXXX
content
During Remove the (NMT 1.0 %)
2.6 Reaction Addition of sample from the Till Production &

CPC
10 ml
2.7 monitoring XXXXXXX reactor through Complies & QC XXXXXXX
Solution Sampler XX
(NMT
3.5%)
During
pH 7- 8
pH Addition of 30-60
3.6
adjustment XXXXXXX
NA NA
min
Production Temp. CPP
25-35ºC
Solution
HPLC- For
After spin
Sample solid Production Information
4.6/ drying the
None

Isolation material from 10 gm Once & Sulphated

5.6 Reaction & QC
Centrifuge Ash- For
Mass
Information

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Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 21 of 26

Method Of Sampling

Quantity of sample

Acceptance criteria
BMR Step No.

Responsibility
Parameter

Frequency

Remarks
Process

HPLC- For
After
Sample solid Production Information
8.6/ XXXXXX completion

None
material from 10 gm Once & Sulphated
10.6 wash of XXXXX & QC
Centrifuge Ash- For
wash
Information
HPLC- For
After
Sample solid Production Information
9.7/ XXXX completion

None
material from 10 gm Once & Sulphated
11.7 Wash of XXXX & QC
Centrifuge Ash- For
wash
Information
During Every

CPP
9.3 Temperature NA NA Production 100 - 105 0C
Drying 60 min
Draw ~3g
Sample the
from Top,
material from tray At time
Middle, and
Loss on dryer interval Production LOD Limit:

None
12.4 Bottom trays ~3g x 3 & QC
drying As per below fig. of 6, 8 NMT: 0.5 %
of TD and
no. 1 & 2 &10 hrs.
then send to
QC.

Draw the one

As per Composite
CCP

14.2 After milling 80 gm Once QC As per BMR

Specification sample from all
drums.

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Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 22 of 26

Method Of Sampling

Quantity of sample

Acceptance criteria
BMR Step No.

Responsibility
Parameter

Frequency

Remarks
Process

Draw sample 80 gm
For from all + Complete
Finished Complete containers make After Productio Analysis as

None
17.1 product composite sample 1.0 kg
analysis & Sifting n & QC per
Analysis for complete for
stability specification
analysis & each
stability batch

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Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 23 of 26
Drawing: Sampling of Tray dryer as per below Figure:
b e
c

d
Fig no. 1. Single Tray

Top

Middle

Bottom
Fig. No. 2 Tray Dryer (TD-304)

13. Packaging and storage:

13.1 Product Containers:
Product shall be packed in transperent Polythene bag [33x66] OR [30x50] Qs then Placed in Black
Polythene bag [33x66] OR [30x50] Qs and then placed in HDPE/Fiber Board container.

13.2 Storage:
Store in a well-closed container protect from light.

14. Validation Acceptance Criteria:

Manufacturing process of (Product Name) is considered as validated if three consecutive batches
Manufactured as per approved Batch Manufacturing record, the following criteria are met.
1. Critical process controls are within defined acceptance criteria.
FORMAT/QA/027/01
Company Logo PROCESS
Company Name and Address VALIDATION
PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 24 of 26
2. Product meets the defined specification.
3. Yield of product is within defined acceptance range

14.1 Revalidation Criteria.

1. Any major change in manufacturing process which may affect the quality of product.
2. Any change in batch size & batch formula.
3. Manufacturing site
4. Any modification in any critical equipment and major modification in utility system.
5. Any change in source of Key starting material.
6. Change in Primary packaging material.

14.2 Critical Process Controls:

Critical process controls for (Product Name) shall conform to predefined acceptance criteria as per
section 12.0

14.3 Yield Acceptance Criteria:

85.71 to 102.85 % on Input of XXXXXXXXX.

14.4 Stability Study:

If acceptance criteria at all the stage of 3 batches are satisfied, the process to be accepted as
validated for manufacturing the product at the site, sequent the validation batches shall be
introduced for complete stability study as per stability protocol.

14.5 Conclusion:
Based on the result of all the 3 batches suitable conclusion will be drawn with respect to the
suitability of proposed process of manufacturing for the (Product Name) conclusion about the
suitability of the validation batches for stability testing could be drown.
14.6 Report Approval:
Process validation data shall be compiled and report shall be prepared by officer or Executive –QA
this report shall be checked by Asst. Manager - QA, Manager - QC, Manager - Production and
approved by Head -QA
15. Changes and deviations:
Any changes or deviations during the process of validation batches shall be documented and
reported in the process validation report and Batch manufacturing Records.

FORMAT/QA/027/01
Company Logo PROCESS
Company Name and Address VALIDATION
PROTOCOL
Title: Validation Protocol
Product Name XXXXXXXX
Documents No. XXXXXXxXX
Type of Validation: Prospective Validation
Department : Quality Assurance Page No.: 25 of 26
16. Validation summary:
In the Process validation report present a summary of validation discussing Stability equipment
suitability, input materials, critical process control parameters, product quality and yield. Draw
appropriate conclusions on the validation and present any recommendations as a result of the
validation including recommendation to correct any deficiencies observed.

17. References:
Sr.
Document Reference
No.
1 Batch Manufacturing Record : XXXXXXXXX
XXXXXXXXXX
2 Specifications and Test Methods for Final product :
XXXXXXXXXXXX

18. Annexure:

Annexure-01 : Training
Annexure-02 : List of standard operating procedures
Annexure-03 : Abbreviations

Annexure-04 : Specification for (Product Name)

FORMAT/QA/027/01
Annexure-01
Annexure-02
 LIST OF STANDARD OPERATING PROCEDURE
S. No. Title of SOP SOP No.
1 Operating procedure for Reactor XXXXXX
2 Operating Procedure For Centrifuge XXXXXXX
3 Operating Procedure For Tray Dryer XXXXXX
4 Operating procedure for Multimill XXXXXX
5 Periodic cleaning Procedure for Dedicated Equipments XXXXXX
6 Process Validation XXXXXX
Annexure-03
 ABBREVIATIONS
S. No. Code Abbreviation
1. BMR Batch Manufacturing Record
2. MFR Master Manufacturing Record
3. RBZ (Product Name)
4. QA Quality Assurance
5. PDL Process Devlopment Lab
6. SSR Stainless Steel Reactor
7. GLR Glass Lined Reactor
8. CF Centrifuge
9. TD Tray Dryer
10. MM Multimill
11. SOP Standard Operating Procedure
12. PPE Personnel Protective Equipment
13. NLT Not Less Than
14. NMT Not More than
15. ETP Effluent Treatment Plant
16. HDPE High Density Polyethylene
17. PR Production
18. COA Certificate of Analysis
19. RT Room Temperature
20. CPC Critical in process control
Annexure-04