Process Validation Protocol
July 26, 2022 | Author: Anonymous | Category: N/A
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Company Logo Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Page No.:
Process Vali alidati dation on Protocol For XXXXXXXXXX
Company Name and Address
1.
FORMAT/QA/027/01
Table ble of Conten tents
PROCESS VALIDATION PROTOCOL
1 of 26
Company Logo Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Page No.:
PROCESS VALIDATION PROTOCOL
2 of 26
1.
Table of Conte Contents... nts.......... ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. ................... .............2 .2
2.
Signatories Signatories...... ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ..........................3 ....................3
3.
Revision Revision status:.. status:......... .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ............. .................4 ..........4
4.
Aim........ Aim............... .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. ................. ......................5 ............5
5.
Purpose...... Purpose............ ............. .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ........................ .........................5 ........5
6.
Scope........ Scope............... .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ............... .............................. ........................5 ..5
7.
Responsibi Responsibility. lity........ .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ..................... ....................5 .....5
8.
Manufactur Manufacturing ing conditions.. conditions......... ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ..............6 ........6
9.
Process Process Equipment’ Equipment’s...... s............ ............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. ................ ............7 ...7
10.
Raw Materials Materials and Packing Packing Materials. Materials........ .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. ................. ........................1 ..............11 1
11 11..
Validation alidation Plan......... Plan................ .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ...........15 .....15
12.
Critical Critical Process Process Controls, Controls, sampling sampling plan and acceptance acceptance criteria:. criteria:........ .............. ............. ............. .............. ............. .....................2 ...............21 1
13.
Packaging Packaging and storage:... storage:......... ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ........................ ..................24 .24
14.
Validation alidation Acceptance Acceptance Criteria: Criteria:....... ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. ......................24 ...............24
15.
Changes and deviations: deviations:...... ............. .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ...................... ....................25 ....25
16.
Validation alidation summary:... summary:......... ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. ................26 .........26
17.
References: References:....... .............. ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ............. ........................ ..........................26 ........26
18.
Annexure:.... Annexure:........... .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. .............. ............................. .......................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 VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Prepared By: Designation Mr. XXXXXXXXX
Page No.:
3 of 26
Signature
Date
Signature
Date
Signature
Date
Signature
Date
Signature
Date
Signature
Date
Signature
Date
Sr Sr.. Executive-PR Exe cutive-PR Reviewed By: Designation Mr. XXXXXXXX Sr. Manager - PR Designation Mr. XXXXXXXXXXX Dy. Manager - PD Designation Mr. XXXXXXXXX Asst. Manager - QC Designation Mr. XXXXXXXXX Manager- EG Designation Mr. XXXXXXXXXX Executive - QA Approved By: Designation Mr. XXXXXXX Asst. Manager - QA 3. Revi Revisi sion on stat status us:: Sr. No.
FORMAT/QA/027/01
Date
Revision
Changes Made
Company Logo
PROCESS VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
1
FORMAT/QA/027/01
13/06/2019
Page No.:
R00
Initial copy
4 of 26
Company Logo Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Page No.:
PROCESS VALIDATION PROTOCOL
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 all a 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. 2. 3. 4.
To execute the batches as per BMR & process validation protocol. protocol. Preparation Preparation of process process validation validation protocol protocol with the help of QA. Compilation of data data related to manufacturing manufacturing area and furnish furnish the same for review. review. Review of protocol protocol and summary summary report. report.
Quality Control Shall be responsible for :
1. 2. 3. 4.
Raw material material and packing packing material material analysis. analysis. Inprocess and finished finished product sampling and analysis as per sampling plan. Collection and review of Inprocess and finished product analysis data. Submission of data / Result Result to QA & production for review & evaluation.
FORMAT/QA/027/01
Company Logo Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Page No.:
PROCESS VALIDATION PROTOCOL
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. 2. 3. 4. 5. 6. 7. 8.
Product name
(Product Name)
Generic name
(Product Name)
Chemical name
XXXXXXXXXXXX
Shelf life
5 years
Storage condition
XXXXXXXXXXXXXXX.
Batch size
XXXXXX kg
Packing ins insttruction
Packing st sty yle
Use
XXXXXXXX
FORMAT/QA/027/01
Company Logo
PROCESS VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Page No.:
7 of 26
9. Proce Process ss Equip Equipme ment’ nt’ss
Sr. Sr. No.
1.
Equipment Name
SS Reactor
Equipment Code
XXXXXXX
Qualification Status & Preventive Maintenance ( Due Date)
Qualification Due Date: XXXXXX Preventive maintenance Due Date: XXXXXXX
Capacity/ MOC/RPM etc.
2.
Glass Lined Reactor
FORMAT/QA/027/01
R-212
Preventive maintenance Due Date: 16 Aug.2019
Purpose
Working Capacity
2000 L MOC SSR RPM 50 Agitator Anchor
Working Qualification Due Date: 20 Oct 2020
Details of Control and Measuring Equipment
VG-R-211/01 Range 760 mm Hg – 0 TI-R-211/01 Range Ra nge 0 to 400⁰C TS-R-211/01 Range Ra nge 0 tto o 200 200⁰C
Sodium hydroxide solution preparation
PG-R-212/01 Range 0 to 7 Kg/cm2 PG-R-212/02 2
Capacity 3000 L MOC GLR RPM 102 Agitator Impeller
Range 0 to 10.6 Kg/cm PG-R-212/03 Range 0 to 4 Kg/cm2 VG-R-212/01 Range 760 mm Hg – 0 TS-R-212/01 Range 0 to 200°C TI-R-212/01 Range 0 to 200°C
Reaction
Company Logo
PROCESS VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Sr. Sr. No.
3.
4.
Equipment Name
Glass Lined Reactor
SS Reactor
Equipment Code
Qualification Status & Preventive Maintenance ( Due Date)
Qualification Due Date: 27 Nov 2019
R-213
R-214
Preventive maintenance Due Date: 22June2019
Qualification Due Date: 06 Dec 2019 Preventive maintenance Due Date: 23 June2019
Qualification Due Date: 20 Oct 2020
5.
Centrifuge
CF-202
Preventive maintenance
Due Date: 22June2019
FORMAT/QA/027/01
8 of 26
Page No.: Capacity/ MOC/RPM etc.
Working Capacity 4000 L MOC GLR RPM 98 Agitator Impeller
Working Capacity 6000 L MOC SSR RPM 60
Details of Control and Measuring Equipment
PG-R-213/01 Range 0 to 7 Kg/cm2 PG-R-213/02 Range 0 to 10.6 Kg/cm2 VG-R-213/01 Range 760 mm Hg – 0
Purpose
Reaction
TS-R-213/01 Range 0 to 200°C TI-R-213/01 Range 0 to 200°C
VG-R-214/01 Range 760 mm Hg – 0 TI-R-214/01 Range 0 to 400 C ⁰
Water Washing
TS-R-214/01 Range 0 to 200 C ⁰
Agitator Anchor
Capacity 48” Dia. MOC SS
RTM-01 Range 200 to 2000 LPH
Isolation
Company Logo
PROCESS VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Sr. Sr. No.
Equipment Name
Equipment Code
Qualification Status & Preventive Maintenance ( Due Date) Qualification Due Date: 20 Oct 2020
6.
Centrifuge
CF-203
Preventive maintenance Due Date:
9 of 26
Page No.: Capacity/ MOC/RPM etc.
Capacity 48” Dia. MOC SS
Details of Control and Measuring Equipment
Purpose
RTM-01 Range 200 to 2000 LPH
Isolation
23Aug 2019 Qualification Due Date: 24 Jan 2020
7.
8.
9.
Tray Dryer
Multimill
Sifter
FORMAT/QA/027/01
TD-303
MM-304
SFR-303
Preventive maintenance Due Date: 20 July2019 Qualification Due Date 07 March 2021 Preventive maintenance Due Date: 16Aug 2019 Qualification Due Date 20 Dec 2019 Preventive maintenance Due Date: 17June2019
Capacity 96 Trays MOC SS
PG-TD-303/01 Range 0 to 7 Kg/cm2 TS-TD-303/01 Range 0 to 200⁰C
Drying
TI-TD-303/01 Range 0 to 200⁰C
Working Capacity 125 Kg/hrs. MOC SS
NA
Milling
NA
Sifting
Mesh Size 0.5 mm Working Capacity 36”. MOC SS Mesh Size 10 mm
Company Logo Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Page No.:
PROCESS VALIDATION PROTOCOL
10 of 26
Details of QC instruments : Sr. Sr. No.
Equipment Name
Equipment ID
Make
Calibration Status
Purpose
Cal. Due date: 18/08/2019
Analysis
1.
HPLC
M/QC/I/003
AGILENT
2.
HPLC
M/QC/I/004
AGILENT
3.
HPLC
M/QC/I/076
AGILENT
4. 5.
HPLC UV Spectrophotom eter
M/QC/I/097
SHIMADZU
M/QC/I/104
Shimadzu
Cal. Due date: 30/06/2019
Analysis Analysis
Analysis
Cal. Due date: 18/06/2019
Analysis
Cal. Due date: 14/06/2019
Analysis
6.
GC
M/QC/I/013
7.
GC
M/QC/I/077
AGILENT
Cal. Due date: 19/06/2019
Analysis
8.
IR
M/QC/I/023
SHIMADZU
Cal. Due date: 09/08/2019
Analysis
9.
Auto Titrator & KF Titrator
M/QC/I/107
Metrohm
Cal. Due date: 21/08/2019
Analysis
10.
Vacuum oven
M/QC/I/017
SHEETAL
Cal. Due date: 02/12/2019
Analysis
11.
Drying oven
M/QC/I/016
Cal. Due date: 02/12/2019
Analysis
12.
Muffle Furnace
M/QC/I/056
Cal. Due date: 02/12/2019
Analysis
13.
Muffle furnace
M/QC/I/079
Cal. Due date: 02/12/2019
Analysis
FORMAT/QA/027/01
PERKIN ELMER
Cal. Due date: 15/08/2019 Cal. Due date: 16/06/2019
PATHAK ELECTRICALS GALAXY SCIENTIFIC EQPT. NA
Company Logo Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
10. 10.1
11 of 26
Page No.:
Raw Raw Mater Materia ials ls and Pack Packing ing Mater Material ialss Raw Ma Material
Sr. Sr. No .
Code
1.
XXXXXXX
XXXXXXX In-house
2.
-
XXXXXXX In-house
Ingredient
Vendor Name
XXXXXXX XXXXXXX
3.
PROCESS VALIDATION PROTOCOL
XXXXXXX
4. 4.
XXXXXXX
5. 5.
XXXXXXX
FORMAT/QA/027/01
Rationale
XXXXXXX
Key Ra Raw material Washing
XXXXXXX XXXXXXX
XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX
XXXXXX X
XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXX X
Spec No
XXXXXXX XXXXXXX XXXXXXX
Solvent for reaction
XXXXXXX Reagent
XXXXXXX
Acid
Company Logo
PROCESS VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Sr. Sr. No .
6 6..
7 7..
10.2 Sr. No.
Code
XXXXXXX
XXXXXXX
Ingredient
XXXXXX X
XXXXXX X
Vendor Name
M/s. Heetu chemicals & alkalies ltd. XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX
Spec No
XXXXXXX
Reagent
Solvent for washing
Packing ing Mate terrials als Code
Ingredient
Vendor Name
XXXXXXX
XXXXXXX
Spec No
Primary packing
XXXXXXX
XXXXXXX
Black Polythene bag (33” x 66”)
XXXXXXX XXXXXXX XXXXXXX XXXXXXX
XXXXXXX
Primary packing
XXXXXXX XXXXXXX XXXXXXX
XXXXXXX FORMAT/QA/027/01
XXXXXXX
Rationale
XXXXXXX
XXXXXXX
02
Rationale
XXXXXXX
XXXXXXX 01
12 of 26
Page No.:
XXXXXXX
Company Logo
PROCESS VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance HDPE full open top drum (120 lit.)
03
04
05
06
07
08
09
10
11
HDPE full XXXXXXX open top drum (60 lit.) Black XXXXXXX Polythene bags (50[L]X30[W]) XXXXXXX
Transparent Polythene bags
XXXXXXX
1200001443
1200001444
Drum CAP – 60 L SEA UN No. HDPE Full Open Drum CAP – 60 L AIR
Secondary packing
XXXXXXX XXXXXXX XXXXXXX
XXXXXXX
XXXXXXX XXXXXXX XXXXXXX XXXXXXX XXXXXXX
XXXXXXX
(50[L]X30[W] ) XXXXXXX XXXXXXX Fiber Board XXXXXXX XXXXXXX Drums (18X28) UN No. HDPE XXXXXXX Drum Capacity 120 L-SEA UN No. HDPE XXXXXXX Drum Capacity 120 L-AIR UN No. HDPE Full Open
13 of 26
Page No.:
XXXXXXX
Primary packing Secondary packing
XXXXXXX
XXXXXXX
Secondary packing
XXXXXXX
XXXXXXX
Secondary packing
XXXXXXX
XXXXXXX
Secondary packing
XXXXXXX
Secondary packing
XXXXXXX
Raw material and packaging material shall confirm to the In-house specifications.
FORMAT/QA/027/01
Primary packing
XXXXXXX
Note:
Secondary packing
Company Logo Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
11.
0
PROCESS VALIDATION PROTOCOL
Page No.:
14 of 26
Valida idatio tion Plan
11.1 Process Details for Manufacturing of (Product Name): 11.1 .1.1 .1
Diss sso olutio tion of XXXXXXX in XXXXXXX:
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.
FORMAT/QA/027/01
Company Logo Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
11.1.3 1.1.3
Page No.:
PROCESS VALIDATION PROTOCOL
15 of 26
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
Company Logo Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Page No.:
PROCESS VALIDATION PROTOCOL
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 R214. 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 (W et 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-XXC 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 process Sample: 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 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 Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Page No.:
PROCESS VALIDATION PROTOCOL
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 Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
FORMAT/QA/027/01
Page No.: Process Flow
PROCESS VALIDATION PROTOCOL
18 of 26
Company Logo Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
11.2
Page No.:
PROCESS VALIDATION PROTOCOL
19 of 26
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 VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
12.
20 of 26
Page No.:
Critica Criticall Proces Processs Control Controls, s, samplin sampling g plan plan and acce acceptan ptance ce crite criteria: ria:
. o N p e t S R M B
r e t e m a r a P
Temperature 1.2
and Time
Temperature 2.5 and Time
2.6 2.7
3.6
4.6/ 5.6
Reaction monitoring
s s e c o r P
During Addition of XXXXXX Solution Stir reaction mass at 4550ºC for 60 min.
NA
NA
During Addition of XXXXXXX
Remove the sample from the reactor through
Solution
Sampler
pH adjustment
During Addition of XXXXXXX Solution
Isolation
After spin drying the Reaction Mass
FORMAT/QA/027/01
g n i l p m a S f O d o h t e M
NA
Sample solid material from Centrifuge
e l p m a s f o y t i t n a u Q
NA
NA
10 ml
y c n e u q e r F
y t i l i b i s n o p s e R
Every 60 Production min
--
Production
a i r e t i r c e c n a t p e c c A
s k r a m e R
P
30-45°C
P C
Temp. 4550ºC and Time 60 min.
P P C
XXXXXXX content (NMT 1.0 %) Production & Till & QC XXXXXXX Complies
C P C
XX (NMT 3.5%) NA
10 gm
pH 7- 8 Temp. 25-35ºC
30-60 min
Production
Once
HPLC- For Production Information & Sulphated & QC Ash- For Information
P P C
e n o N
Company Logo
PROCESS VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
. o N p e t S R M B
8.6/ 10.6
r e t e m a r a P
XXXXXX wash
s s e c o r P
After completion of XXXXX
n g i l p m a S f O d o h t e M Sample solid material from Centrifuge
e l p m a s f o y t i t n a u Q
10 gm
y c n e u q e r F
XXXX Wash
9. 9.3 3 Tempe empera ratture ure
12.4
14.2
Loss on drying
a i r e t i r c e c n a t p e c c A
s k r a m e R
Once
e n o N
e n o N
After completion of XXXX wash
Sample solid material from Centrifuge
10 gm
Once
HPLC- For Production Information & Sulphated & QC Ash- For Information
During Drying
NA
NA
Every 60 min
Production 100 - 105 0C
P P C
Draw ~3g from Top, Middle, and
Sample the material from tray
At time
As perdryer below fig. ~3g x 3 no. 1 & 2
interval of 6, 8 &10 hrs.
Production LOD Limit: & QC NMT: 0.5 %
e n o N
Bottom trays of TD and then send to QC.
As per After milling Specification
FORMAT/QA/027/01
y t i l i b i s n o p s e R
HPLC- For Production Information & Sulphated & QC Ash- For Information
wash
9.7/ 11.7
21 of 26
Page No.:
Draw the one Composite sample from all drums.
80 gm
Once
QC
As per BMR
P C C
Company Logo
PROCESS VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
. o N p e t S R M B
r e t e m a r a P
Finished 17.1 product Analysis
FORMAT/QA/027/01
s s e c o r P
For Complete analysis & stability
22 of 26
Page No.:
n g i l p m a S f O d o h t e M Draw sample from all containers make composite sample for complete analysis & stability
e l p m a s f o y t i t n a u Q
y c n e u q e r F
y t i l i b i s n o p s e R
a i r e t i r c e c n a t p e c c A
s k r a m e R
80 gm + 1.0 kg for each batch
After Sifting
Productio n & QC
Complete Analysis as per specification
e n o N
Company Logo
PROCESS VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
23 of 26
Page No.:
Drawing: Sampling of Tray dryer as per below Figure: b e
c
a
d Fig no. 1. Single Tray
Top
Middle
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::
Bottom
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 Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
Page No.:
PROCESS VALIDATION PROTOCOL
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. 2. 3. 4. 5. 6. 14 14.2 .2
Any major major change in manufac manufacturin turing g process which may may affect affect the quality quality of product. product. Any chan change ge in batc batch h size size & batch batch form formula ula.. Manu Manufa fact ctur urin ing g site site Any modificati modification on in any critical critical equipment equipment and major modifi modification cation in utilit utility y system. system. Any chang changee in source source of Key star starti ting ng materi material. al. Change Change in Prim Primary ary packa packagin ging g materi material. al.
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 val idated 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 and d 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 VALIDATION PROTOCOL
Company Name and Address Title:
Validation Protocol
Product Name
XXXXXXXX
Documents No.
XXXXXXxXX
Type of Validation:
Prospective Validation
Department :
Quality Assurance
16 16..
Valid alidat atio ion n sum summ mary: 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. No. 1
2
18.
25 of 26
Page No.:
Document
Reference
Batch Ma Manufacturing Re Record
:
XXXXXXXXX XXXXXXXXXX
Speci Specifi ficat catio ions ns and Tes estt Meth Method odss for for Final Final prod produc uctt
:
XXXXXXXXXXXX
Annexure:
Annexure-01
: Training
Annexure-02
: List of standard operating procedures
Annexure-03
: Abbreviations
Annexure-04
:
FORMAT/QA/027/01
Specification for (Product Name)
Annexure-01
Annexure-02
LIST OF STANDARD OPERATING PROCEDURE S. No.
Title of SOP
SOP No.
1
Ope perrating proc oceedure for Reactor
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
XXXXXX
Annexure-03
ABBREVIATIONS S. No.
Code
Abbreviation
1.
BMR
Batch Manufacturing Record
2.
MFR
Master Manufacturing Record
3.
RBZ
(Product Name)
4. 5.
QA PDL
Quality Assurance 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
17.
PR
18.
COA
19.
RT
20.
CPC
High Density Polyethylene Production Certificate of Analysis Room Temperature Critical in process control
Annexure-04
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