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.: 1 of 26

Process Vali
alidati
dation
on

Protocol For
XXXXXXXXXX

Company Name and Address

1. Tabl
blee of Conten
tents
Follow Pharma Broadcast
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.: 2 of 26

1. Table of Conte
Contents...
nts..........
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2. Signatories
Signatories......
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3. Revision
Revision status:..
status:.........
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4. Aim........
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5. Purpose......
Purpose............
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6. Scope........
Scope...............
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7. Responsibi
Responsibility.
lity........
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.....5

8. Manufactur
Manufacturing
ing conditions..
conditions.........
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........6

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

10. Raw Materials

Materials and Packing
Packing Materials.
Materials........
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........................1
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1

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

12. Critical
Critical Process
Process Controls,
Controls, sampling
sampling plan and acceptance
acceptance criteria:.
criteria:........
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.....................2
...............21
1

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

14. Validation
alidation Acceptance
Acceptance Criteria:
Criteria:.......
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15. Changes and deviations:

deviations:......
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....25

16. Validation
alidation summary:...
summary:.........
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17. References:
References:.......
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18. Annexure:....
Annexure:...........
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.......................26
.26

2. Si
Sign
gnat
ator
orie
iess
This document contains 25 pages and is prepared, reviewed and approved by following persons:

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.: 3 of 26
Prepared By:
Designation Signature Date
Mr. XXXXXXXXX

Sr
Sr.. Executive-PR
Exe cutive-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. Revi
Revisi
sion
on stat
status
us::

Sr. No. Date Revision Changes Made

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.: 4 of 26

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.: 5 of 26
4. Aim
The aim of this valida
validati
tion
on protoc
protocol
ol is to provid
providee the validati
validation
on of (Product Name) manufacturing
process as per in line with BMR No. XXXXXXXXXX.

5. Purpo
rpose
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 alla ll 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. Resp
Respon
onsi
sibi
bili
lity
ty
Functional responsibility is with the validation team comprising of:
 Quality Assurance Shall be responsible for :
1. Approval
Approval & training
training of validation
validation protocol, review
review of the data compiled,
compiled, review of deviation
deviation (if
any), monitoring of the process as per process parameter & monitoring of withdrawal of validation
sample.
2. Review of the facility,
facility, equipment qualification & utility validation report.
3. cGMP compliance
compliance during the manufacturing
manufacturing process review & evaluation of data /Result generated
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.
protocol.
2. Preparation
Preparation of process
process validation
validation protocol
protocol with the help of QA.
3. Compilation of data
data related to manufacturing
manufacturing area and furnish
furnish the same for review.
review.
4. Review of protocol
protocol and summary
summary report.
report.
 Quality Control Shall be responsible for :
1. Raw material
material and packing
packing material
material analysis.
analysis.
2. Inprocess and finished
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
Result to QA & production for review & evaluation.

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.: 6 of 26
 Process Development Shall be responsible for:
1. To monitor activities related
related to execution of the process vali
validation
dation in coordination with Production
and QA.
 Engineering Shall be responsible for:
1. To review the protocol and provide support with equipment’s,
equipment’s, facility and manufacturing
condition.

8. Manufact
Manufacturi
uring
ng conditi
conditions:
ons:

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 ins
insttruction Packing st
sty
yle
8.
Use XXXXXXXX

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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.: 7 of 26

9. Pr
Proce
ocess
ss Eq
Equip
uipme
ment’
nt’ss
Qualification
Status & Capacity/
Sr.
Sr. Equipment Equipment Details of Control and
Preventive MOC/RPM Purpose
No. Name Code Measuring Equipment
Maintenance etc.
( Due Date)

Working
Capacity
Qualification
Due Date:
XXXXXX MOC
XXXXXXX SSR
1. SS Reactor
Preventive solution
RPM preparation
maintenance
Due Date:
XXXXXXX Agitator
Anchor

Working
Qualification 2

Due Date: Capacity

Glass Lined
2. Reaction
Reactor Preventive
maintenance RPM
Due Date:
Range
Agitator
Impeller
Range

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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/ Details of Control
Sr
Sr.. Equipment Equipment
Preventive MOC/RPM and Measuring Purpose
No. Name Code
Maintenance etc. Equipment
( Due Date)

Working
Qualification Capacity
Due Date:

Glass Lined MOC

3. Preventive
Reactor maintenance
Due Date: RPM

Agitator
Impeller

Qualification
Working
Due Date:
Capacity

mParienvteen
ntain
vcee MOC
4. SS Reactor Due Date: 2 SSR

RPM

Qualification Agitator
Due Date: Anchor

Preventive
maintenance
Capacity

5. Centrifuge
MOC
SS

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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
Sr.. Equipment Equipment Details of Control and
Preventive MOC/RPM Purpose
No. Name Code Measuring Equipment
Maintenance etc.
( Due Date

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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.: 10 of 26

Details of QC instruments :
Sr.
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 30/06/2019 Analysis
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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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.: 11 of 26

10. Raw
Raw Mater
Materia
ials
ls and Pack
Packing
ing Mater
Material
ialss
10.1 Raw Ma
Material
Sr.
Sr.
No Code Ingredient Vendor Name Spec No Rationale
.
XXXXXXX Key Ra
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.
4. XXXXXXX XXXXXXX XXXXXXX Reagent
XXXXXXX
XXXXXXX
5.
5. XXXXXXX XXXXXX XXXXXXX XXXXXXX Acid
X XXXXXXX
XXXXXXX
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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.: 12 of 26
Sr.
Sr.
No Code Ingredient Vendor Name Spec No Rationale
.
M/s. Heetu chemicals & alkalies ltd.
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX XXXXXXX
XXXXXXX
XXXXXXX
XXXXXX
6
6.. XXXXXXX XXXXXXX Reagent
X
XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX XXXXXXX
XXXXXXX
XXXXXXX
XXXXXXX Solvent
XXXXXX
7
7.. XXXXXXX XXXXXXX for
X
XXXXXXX washing
XXXXXXX
XXXXXXX
XXXXXXX

10.2 Packing
ing Mate
terrials
als
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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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.: 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
Primary
05 XXXXXXX Polythene bags XXXXXXX
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.

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.: 14 of 26
11. 0 Valida
idatio
tion Plan
11.1 Process Details for Manufacturing of (Product Name):

11.1
.1.1
.1 Diss
sso tion of XXXXXXX in XXXXXXX:
olutio
Apply vacuum to the reactor R-212 / R-213 and charge XXXX L XXXXX in to reactor.
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
ST-207 by gravity
gravity..
Charge slowly hydrochloric acid XXX Kg at XXXX°C in R-212/R-213 under
u nder 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.
Clear
11.1.2
1.1.2 Prep
Prepar
arati
ation
on of
of XXXX
XXXXXX
XXXX
XXX
X Solut
Solution
ion::
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.
min. Withdraw
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
1.1.3 Prepa
Preparati
ration
on of XXXXXX
XXXXXXXXX
XXXXXX
XXX Solut
Solution
ion in to reac
reactor
tor & pH ad
adjust
justmen
ment:
t:
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
reactor.. Chill solution to XX

– XX C. Transfer the above chilled caustic solution to receiver V-208A/V-213.

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
1.1.4 Isolatio
Isolation
n of the
the Crude
Crude Produc
Productt by Centr
Centrifug
ifugee (CF-202
(CF-202 & CF-203)
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
(Wet cake) in HDPE drums
lined with new polybag.
po lybag. Transfer the material to Reactor area for slurry.
slurry.

11.1.5
1.1.5 Prep
Prepar
arati
ation
on of Slu
Slurr
rry
y in
in Reac
Reacto
tor:
r:

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.
properly. Heat the reaction mixture at
XX-XX°C & Stir for XX min.

11.
1.1.
1.6
6 Hot
Hot Pur
Purif
ifie
ied
d wat
water
er
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
1.1.7 Isolatio
Isolation
n of the Produ
Product
ct in Centrifu
Centrifuge
ge & water
water was
wash:
h:
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
FORMAT/QA/027/01
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Title: Validation Protocol
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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.
receiver. Drain the ML to ETP.
ETP. Wash
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
ETP..

11.1.8
1.1.8 Washing
ashing with
with Fresh
Fresh XXXX
XXXXXX
XXX
X :
Wash the cake in centrifuge with fresh XXXXX from CFT-203
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
Quantity
the centrifuge and allow to stop completely. XX-XX min for relaxation then Unload the product
(Wet
(Wet Cake) in HDPE drums lined with new polybag. Transfer the material to Tray Dryer TD-303for

drying.

11.1.9
1.1.9 Drying
Drying of
of the (Produc
(Productt Name)
Name) in Tray Drye
Dryerr (T
(TD-30
D-303):
3):
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.
min. and record
record the temp
temp detail
details.
s. Cool
Cool the product
product at Room
Room Tempera
emperatur
ture.
e.
Unload the dried product in HDPE drums lined with polybag.

11.1.10
11.1.10 Milling of
of (Product
(Product Name)
Name) (MM-304):
(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
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
1.1.11 In process Sample: Send the In process Sample intimation note given to QC for composite sample
process Sample:
of milled (Product Name) for Description, color value &pH.

11.1.12
1.1.12 Siftin
Sifting
g (SFR-30
(SFR-303):
3):
Place the HDPE/Fibre board drum lined with poly bag below the outlet no
nozzle
zzle of sifter for collecting
the sifted material. Switch ON the Sifter and slowly charge the material in to the Sifter by SS scoop.
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.: 17 of 26
Continue the sifting operation till batch quantity complete. Check
Ch eck the integrity of sieve visually after
completion of sieving. Integrity: Satisfactory / Not Satisfactory.
Satisfactory.

Note:
If the integrity is not satisfactory,
satisfactory, replace it with a new one and sieve the entire
en tire batch quantity again.
11.1.
1.1.13
13 Pack
Packag
agin
ing:
g:

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.
Qty

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.: 18 of 26
Process Flow

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.: 19 of 26

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.

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.: 20 of 26
12. Critica
Criticall Proces
Processs Control
Controls,
s, samplin
sampling
g plan
plan and acce
acceptan
ptance
ce crite
criteria:
ria:

g el
nil a
.
o p
p y rei
m ti t
N li
re ss m
a sa y
c rci s
p
et et ec S f n si
b rk
f o e ec a
S m o y u n
R
a
r r
P
O ti q
er p
o n
a em
a d t se t R
M P o n F p
B h a R ec
et u c
M Q A

During
Temperature P
Addition of Every 60
1.2 and XXXXXX NA NA min Production 30-45°C P
C
Time
Solution

Stir reaction Temp. 45-

Temperature P
mass at 45- Production 50ºC and P
2.5 and NA NA --
50ºC for 60 Time 60 C
Time
min. min.
XXXXXXX
content
During Remove the (NMT 1.0 %)
2.6 Reaction Addition of sample from the Till Production & C
10 ml P
2.7 monitoring XXXXXXX reactor through Complies & QC XXXXXXX C

Solution Sampler XX
(NMT
3.5%)
During
pH 7- 8 P
pH Addition of NA 30-60 Production P
3.6 NA Temp.
adjustment XXXXXXX min C
25-35ºC
Solution
HPLC- For
After spin
Sample solid Production Information e
4.6/ drying the 10 gm n
Isolation material from Once & QC & Sulphated o
5.6 Reaction N
Centrifuge Ash- For
Mass
Information

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.: 21 of 26

nilg el a
.
o p
p y rei
m ti t
N re m y li rci s
ss a sa c
p
et et ec S f n si
b rk
f o e ec a
S m o y u n
R
a
r r
P
O ti q
er p
o n
a em
d t t
M
a
P o n
a F es p R
B h R ec
et u c
M Q A

HPLC- For
After
Sample solid Production Information e
8.6/ XXXXXX completion 10 gm n
material from Once & QC & Sulphated o
10.6 wash of XXXXX N
Centrifuge Ash- For
wash Information
HPLC- For
After
Sample solid Production Information e
9.7/ XXXX completion 10 gm n
material from Once & QC & Sulphated o
11.7 Wash of XXXX N
Centrifuge Ash- For
wash
Information
During Every P
9.
9.3
3 Tempe
empera
ratture
ure NA NA Production 100 - 105 0C P
Drying 60 min C

Draw ~3g
Sample the
from Top,
material from tray At time
Middle, and Production e
n
12.4 Loss on
drying Bottom trays below fig. ~3g x 3
As perdryer interval
of 6, 8 & QC LOD Limit:
NMT: 0.5 % o
N
of TD and
no. 1 & 2 &10 hrs.
then send to
QC.

Draw the one

As per Composite P
14.2 After milling 80 gm Once QC As per BMR C
Specification sample from all C
drums.

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.: 22 of 26

nilg el a
.
o p
p y rei
m ti t
N re m y li rci s
ss a sa c
p
et et ec S f n si
b rk
f o e ec a
S m o y u n
R
a
r r
P
O ti q
er p
o n
a em
d t t
M
a
P o n
a F es p R
B h R ec
et u c
M Q A
Draw sample 80 gm
For from all + Complete
Finished Complete containers make After Productio e
1.0 kg Analysis as n
17.1 product analysis & composite sample Sifting n & QC o
Analysis stability for complete for per
specification N
analysis & each
stability batch

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.: 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
13.. Pack
Packag
agin
ing
g and
and st
stor
orag
age:
e:
13
13.1
.1 Prod
Produc
uctt Cont
Contai
aine
ners
rs::
Product shall be packed in transperent Polythene bag [33x66] OR [30x50] Qs then Placed in Black
Polythene bag [33x66] OR [30x50]
[30x5 0] Qs and then placed in HDPE/Fiber Board container.

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

14. Validat
alidation
ion Acce
Accepta
ptanc
ncee C
Cri
riter
teria:
ia:
Manufacturing process of (Product Name) is considered as validated
v alidated if three consecutive batches
Manufactured as per approved Batch Manufacturing record, the following criteria are met.
1. Critical
Critical process
process control
controlss are within
within defined
defined acceptance
acceptance criteria
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
Product meets
meets the
the defined
defined specifi
specificat
cation
ion..
3. Yield of
of product
product is
is within
within defined
defined accepta
acceptance
nce range
range

14
14.1
.1 Reval
Revalid
idati
ation
on Crite
Criteri
ria.
a.
1. Any major
major change in manufac
manufacturin
turing g process which may
may affect
affect the quality
quality of product.
product.
2. Any chan
change
ge in batc
batchh size
size & batch
batch form
formulaula..
3. Manu
Manufa
fact
ctur
urin
ing
g site
site
4. Any modificati
modification
on in any critical
critical equipment
equipment and major modifi
modification
cation in utilit
utility
y system.
system.
5. Any chang
changee in source
source of Key star
starti
ting
ng materi
material.
al.
6. Change
Change in Prim
Primary
ary packa
packagin
ging
g materi
material.al.

14
14.2
.2 Crit
Critic
ical
al Proc
Proces
esss Cont
Contrrols:
ols:
Critical process controls for (Product Name) shall conform to predefined acceptance criteria as per
section 12.0

14
14.3
.3 Yield
ield Acce
Accept
ptan
ance
ce Crit
Criter
eria
ia::
85.71 to 102.85 % on Input of XXXXXXXXX.

14.4 Sta
tab
bility
lity Study:
If acceptance criteria at all the stage of 3 batches are satisfied, the process to be accepted as
valida
validated
ted for manufa
manufactu
cturin
ring
g the product
product at the sit site,
e, sequent
sequent the valida
validatio
tion
n batches
batches shall
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 Repor
ortt Appr
pro
oval:
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
15.. Chang
hanges
es an
andd dev
devia
iati
tion
ons:
s:
Any changes
changes or deviati
deviations
ons during
during the proces
processs of valida
validatio
tion
n batches
batches shall be docume
documente
nted
d 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
16.. Valid
alidat
atio
ion
n sum
summmary:
ary:
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 Ma
Manufacturing Re
Record : XXXXXXXXX
XXXXXXXXXX

2 Speci
Specifi
ficat
catio
ions
ns and Tes
estt Meth
Method
odss for
for Final
Final prod
produc
uctt : 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 Ope
perrating proc
oceedure for Reactor XXXXXX
2 Operating Procedure For Centrifuge XXXXXXX
3 Operating Procedure For Tray Dryer XXXXXX
4 Ope
perrating proc
oceedure 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