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PROTOCOL

FOR

WATER SYSTEM VALIDATION

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INDEX

Sr. No. Table content Page No.

Cover Page 1 of 20
Index 2 of 20
1.0 Approval of Water system validation Protocol 3 of 20
2.0 Objective 4 of 20
3.0 Scope 4 of 20
4.0 Responsibility 5 of 20
5.0 Material, Instruments and documents 5 of 20
5.1 Chemical / reagent used for validation 5 of 20
5.2 Reference documents used for validation 6 of 20
5.3 System/ Equipment Description 7-8 of 20
6.0 Procedure 9 of 20
6.1 Test Plan for Water system validation 9-10 of 20
6.2 Specification For Validation 10 of 20
6.3 STP For Validation 10 of 20
7.0 Sampling / Analysis Program For Water System Validation 10 of 20
7.1 Sampling Preparation Procedure 10 of 20
7.2 Sampling Location 11 of 20
7.3 Sampling Procedure 11 of 20
7.4 Sampling / Testing Schedule 12-13 of 20
8.0 Monitoring & Controlling Of Water System 14 of 20
9.0 Training Program For Personnel Performing Water System Validation 15 of 20
10.0 Acceptance Criteria 16-17 of 20
11.0 Data recording 17-19 of 20
12.0 Deviation Report 19 of 20
13.0 Water system validation report 20 of 20
14.0 Evaluation 20 of 20
15.0 Conclusion 20 of 20
16.0 Re-qualification 20 of 20

1.0 APPROVAL OF WATER SYSTEM VALIDATION PROTOCOL

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The protocol has been prepared, checked and approved for implementation by the
undersigned:

DEPARTMENT NAME DESIGNATION SIGNATURE DATE

PREPARE
D BY

DEPARTMENT NAME DESIGNATION SIGNATURE DATE

Production

Production

CHECKED Production
BY

Project & Plant

Engineering

Quality Control

Production

DEPARTMENT NAME DESIGNATION SIGNATURE DATE

APPROVE
D BY Quality
Assurance

2.0 OBJECTIVE

The objective of Water System Validation Protocol is as under:

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 Water System Validation protocol will be planned and ensuring that the particular system
will consistently produce water of predictable quality when operated in the prescribed manner.

 Establishing the documented evidence which provides a high degree of assurance that
water generation and distribution system consistently produce water for injection meeting
its predetermined specifications and quality attributes.

 Water System Validation protocol to provide evidence of when, how and by whom the work
was performed, and a record of what results were obtained.

 The objective of the protocol is to provide a rigorous testing to demonstrate the

effectiveness and reproducibility of the total, integrated system.

 It will include the description of the system, specifying its acceptable ranges and limits and
contain schematics of the water system and location of sampling valve should be evident on the
drawing of the system layout.

 If any variation is observed between the set acceptance criteria and the actual data
obtained, then same should be explained reasonably.

 The Quality assurance head and department head shall decide whether deviation is
acceptable or not. If deviation is acceptable and it does not impact the quality of WFI and
Performance of machine, the Water system validation will be continued. If deviation is not
acceptable and it has impact on the quality of WFI, Quality assurance head and department
head will take necessary corrective action for correctness.

3.0 SCOPE:

The scope of this water system validation is to check whether the water for Injection
produced meets the specifications.

The detail of equipment is as under:

Name of Process Water System Validation

Location

Equipment UID

4.0 RESPONSIBILITY

DEPARTMENT DESIGNATION RESPONSIBILITY

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Will prepare Water system validation Protocol

Quality Assurance Assistant Manager & Report as per the guideline of relevant SOP
and Validation Procedure
An execution team will be made to execute
Quality Assurance, Officer / Microbiologist/ the Water system validation as per the
Automation & Analytical chemist /Sr. protocol and testing of samples and analyse
Production Engineer the data and preparation of Water system
validation report.
Quality Control Will review the Water system validation
Manager / Sr.
Maintenance & Quality protocol for correctness, completeness, and
Engineer/ DGM
Assurance technical excellence.

Head of Department, Will approve the Water system validation

Quality Assurance
QA (SGM) protocol.

5.0 MATERIALS, INSTRUMENTS AND DOCUMENTS

5.1 CHEMICAL / REAGENT USED FOR VALIDATION

S.
Material Name Batch No. Used For Verified by (QA)
No.
For BET Testing
1.
(LAL, LRW & CSE)
Cellulose nitrate membrane
2.
(0.45µ)
3. SCDA Media

4. SCDM Media

5. Macconkey Broth

6. Macconkey Agar

7. Cetrimide Agar

8. Rappaport vassiliadis broth

Xylose
9.
lysine deoxycholate agar
10. Mannitol Salt Agar

5.2 REFERENCE DOCUMENTS USED FOR VALIDATION

S. Document
Title Revision No. Verified by (QA)
No. No.
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1. Validation procedure QP/QAD/5.25 00

SP/RM/QC/
2. Specification of Raw and RO water 01
5.10
STP/RM/QC/
3. Test Procedure of Raw water 00
5.10
STP/RM/QC/
4. Test Procedure of RO water 01
5.09
Specification of Purified and Water SP/RM/QC/
5. 01
for Injection water 5.11
Test Procedure of Purified and Water STP/RM/QC/
6. 01
for Injection water 5.11
7. TOC Analyzer WI/QC/28 03

8. pH Meter WI/QC/5.02 00

9. Conductivity Meter WI/QC/5.01 00

5.3 INSTRUMENTS /EQUIPMENTS USED FOR VALIDATION

S. Instrument/ Equipment Calibration / Verified

Instrument/Equipment
No. No. Validation date by (QA)

1. Conductivity Meter LAB/CM/IMT/005

2. pH Meter LAB/PH/IMT/004
3. Analytical Balance LAB/WB/IMT/006
4. Hot Plate LAB/HP/IMT/007
5. Heating Block LAB/HB/IMT/003
6. Lab Autoclave LAB/AUT/IMT/010

7. BOD Incubator-I (30- LAB/BOD/IMT/002

35˚C)
8. BOD Incubator-II (20- LAB/BOD/IMT/003
25˚C)
9. Drying Oven LAB/HAO/IMT/020
10. TOC Analyzer LAB/TOC/IMT/31
11. Micropipettes and Tips NA

12. Depyrogenated Test NA

Tubes
13. Conical Flask NA
14. Test Tubes NA

15. Sterilized assembly and NA

filters
16. Metallic Loop NA

5.4 SYSTEM/ EQUIPMENT DESCRIPTION

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The WFI generation system is multi columns distill plant designed on the basis of
falling film principle. It has 4 columns and a top condenser. The columns are connected
in series. Each column has innermost evaporators (shell and tube heat exchangers, an
intermediate separator, and an outer column). The condenser is a shell and tube
design. The first column is heated with boiler steam and remaining columns are using
the intrinsic heat to supplement consumption needs of the heating energy.

The multi column distilled water system works on the principle of inter-stage heat
exchanger, drastically reduce the consumption of heating energy and cooling water. It
thus enables production of large scale pyrogen free sterile distillate at a fraction of the
cost involved in the conventional system.
The control panel consists of fully automatic operation panel included in the unit so as
to enable automatic operation. High purity Flow Diversion valve & air vent valve
provided in multicolumn are pneumatically operated.

5.4.1 IN PUT PARAMETERS FOR WFI GENERATION UNIT

 Feed Water: De-ionized water with Maximum Conductivity of 5.0 µS.

 Cooling Water
 Steam: The boiler supply dry and saturated steam at 4 ± 1 Kg/cm 2 pressure
and 150 ± 5 °C temperatures.
 Air Pressure: Required for operating of valves. Pressure 4 to 5 kg/cm2.
 The system is provided with 415 V ±5 %, 50 Hz, 3Phase power supply .

5.4.2 SCHEMATIC DIAGRAM OF WATER SYSTEM

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Remove
organism &
remaining
Reverse hardness De-
RO water
Raw Osmosis Mineralized
Storage
Water Unit Water Unit
(Highly
Tank (Ion Exchange
Pressurized Process)
water passed
SP- through Semi- SP-
01 permeable) 02 SP-
membrane 03
SP
-
Removal of 04
Removal of Non volatile TOC and
and Micro-organism & Micro-
Transfer the whole WFI in organism
Storage Tank
WFI WFI
Storage/Distr
SP-05 SP-04
Generatio DM Water
ibution Tank n Unit Storage
(Maintain 80˚C (Distillation Tank
Temperature of Process)
SP- WFI) SP- SP-
07 06A 05

SP-
Return WFI Distribution
10 loop to WFI storage tank

Distribution loop User Point-I User Point-II

of WFI to PFS area
(Mixing (Filling
Area) Area)

SP-08 SP-09
Supply of WFI to
mixing tank for
solution
preparation

Remarks: SP : Sampling Point

6.0 PROCEDURE

6.1 TEST PLANS FOR WATER SYSTEM VALIDATION

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The Water system validation will be carried out as follows:

6.1.1 PHASE 1: VALIDATION FOR 2 WEEKS:

The objective of Phase - 1 study will be:
 Phase –I shall be taken for two weeks to establish the operating parameters and
procedures.
 Water system shall continuously run so that system operates stable and within
the required ranges.
 To ensure that water meets the quality consistently as per the specification.
 To collect the samples from each unit in treatment of water system before and
after delivering of water.
 Daily water samples are taken downstream from each unit in the treatment
system and form each point of use in the holding /distribution system to
assess the chemical and microbiological quality of the water. Pathogen testing
will be conducted after getting the results of test. Pathogen test will be
conducted three times in this phase i.e. start, middle & end of the phase.
 Data from the daily samples taken over a 2 weeks period should be used to
develop SOP’s, appropriate maintenance, and cleaning protocols and
analytical schedules for each unit in the system.
 WFI will be sampled and tested from storage tank and distribution lines for
last days Phase -1, and then it should be released for Phase-2.

6.1.2 Phase 2: Validation for 2 week:

The objective of Phase - 2 studies will be:

 Daily sampling is continued in phase 2 for another 2 week from the sampling
point’s mentions in table-1 below and tests are conducted as per specification
SP/RM/QC/5.11. During this phase, the water system is operated according to
the protocols and schedules developed during phase 1.
 Short-term control phase usually taking 2 weeks, serves to demonstrate
consistent
operation within the established ranges.
 To ascertain that the system delivers the quality of water for injection as per
alert/ action limit.
 The data can also be used as the base line data for trend analysis of the system.
 Before water is permitted to be used for pharmaceutical purposes, an interim
qualification report is required, documenting the successful completion of Phase
2.
 However, water can also be used for pharmaceutical purposes during this phase,
provided that the respective batches are not released until the interim
qualification report has been finalized.
 If the results obtained from monitoring are satisfactory as per limits specified in
SP/RM/QC/11, the multi-column distillation plant is said to be validated and
WFI produced from it can be taken for Phase -3 validations.
6.1.3 Phase 3: Validation for 1 year including Phase 1 and Phase 2

The objective of Phase – 3 studies will be:

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 Phase 3 of the validation program consists of reviewing the routine

monitoring data. This will demonstrate that the phase-1 and phase-2 are
adequate to handle variations in the quality both chemically and
microbiologically of all the incoming of feed water.
 At the end of phase 2 the sampling schedule changes to that of routine
monitoring.
 Sampling for Chemical testing and Microbial testing to be done randomly
from any sampling points so that Sampling point (SP-1 to SP-10) must be
covered within a week Pathogen testing will be conducted after getting the
results of test. Pathogen test will be conducted twice in a month in third
phase.
 For Purified water systems, microbial testing should be performed on each
point of use at least weekly.
 The water generated during the second and third validation phases can be
used to manufacture drug product.
 Daily routine monitoring of WFI shall be conducted in accordance with
SP/RM/QC/5.11.
 Trend analysis shall be done after completion of phase.
 The data obtained at the end of each phase shall be analyzed and corrective
action will be taken, if required.
 At the end of phase of 3, if all data indicate that the water system when
operated according to its SOP consistently produces water that meets its
specification the water system can be considered validated.

6.2 SPECIFICATION FOR VALIDATION

Follow the SP/RM/QC/5.11, Rev. No.-00. SP/RM/QC/5.10, Rev. No.-01

6.3 STANDARD TEST PROCEDURE FOR VALIDATION

Follow the STP/RM/QC/5.10, Rev. No.-00, STP/RM/QC/5.11, Rev. No.-01

7.0 SAMPLING / ANALYSIS PROGRAM FOR WATER SYSTEM VALIDATION:

7.1 SAMPLING PREPARATION PROCEDURE:

 Prepare the required quantity of containers for the scheduled water samples,
ensuring that each sample container is identified with the date, time in taking the
sample.
 For Microbiological samples, water is collected in sterilized flask.
 For Microbiological samples, spray the port with a 70 % isopropyl alcohol.
 For Microbiological samples, wear the latex gloves when handling sample
containers.
 For Microbiological samples, attach a length of sterile tubing to the sampling
port, if possible. In all cases, flush the port being sampled to drain for at least 30
sec.
 Collect required quantity of the container for sampling, Ensure the container is
properly identified, and remove to testing laboratory.
 For chemical samples, cover the conical flask with airtight stopper or with
aluminum foil to avoid Environmental contamination and mention the name of
sample on conical flask with permanent marker.
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7.2 SAMPLING LOCATION

Sampling points in pretreatment of water system, during water treatment, system, WFI
storage, and distribution system of WFI.

Table-1
Sampling
S. No. Location
Numbers
Pretreatment of Water system
1. SP-01 Raw water- Storage Tank- Top Floor
2. SP-02 Outlet Point at RO water Plant- Top Floor

3. SP-03 Outlet Point at RO water Tank- Top Floor

During water treatment system

4. SP-04 Outlet Point of DM water Plant - Top Floor

5. SP-05 Outlet Point of DM water Tank- Top Floor
6. SP-06A Outlet Point of WFI Generation- Top Floor

7. SP-07 Outlet Point of WFI Storage Tank- Top Floor

Distribution system of WFI

8. SP-08 User point-I, Mixing Area-Clean room- PFS

9. SP-09 User point-II, in Filling Area - PFS

10. SP-10 Return WFI distribution loop to WFI storage tank

7.3 SAMPLING PROCEDURE

7.3.1 PRETREATMENT
The pretreatment system will be sampled and tested as follow:
 The raw water from sample port, SP-01 will be sampled and tested as per
schedule for particular content.
 Water from sample port, SP-02 after reverse osmosis process, will be
sampled and tested as per schedule for particular content.
 Water from sample port, SP-03 from reverse osmosis tank, will be
sampled and tested as per schedule for particular content.
7.3.2 MANUFACTURING INTERMEDIATE TREATMENT
The manufacturing intermediate treatment system will be sampled and tested
as follows:
 Water from sample port, SP-04 after De-mineralized water, will be
sampled and tested as per schedule for particular content.
 Water from sample port, SP-05 from De-mineralized water tank, will be
sampled and tested as per schedule for particular content.
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 Water from sample port, SP-06A after WFI generation unit, will be
sampled and tested as per schedule for particular content.
 Water from sample port, SP-07 after WFI storage tank in maintenance,
will be sampled and tested as per schedule for particular content.
 Water from sample port, SP-08 from user point-I in mixing area, will be
sampled and tested as per schedule for particular content.
 Water from sample port, SP-09 from user point-II in Filling Area, will be
sampled and tested as per schedule for particular content.
 Water from sample port, SP-10 from return WFI distribution loop, will be
sampled and tested as per schedule for particular content.
7.4 SAMPLING / TESTING SCHEDULE
7.4.1 SAMPLING SCHEDULE FOR PHASE - 1 VALIDATION

S. Sample Quantity
Sampling Test to be Frequenc
No Duration
Point No. conducted Microbiologic y
. Chemical
al
Raw Water, SP-
1. Refer SP/RM/QC/5.10 200 ml 100 ml For 2 weeks Daily
01
RO Water Plant,
2. Refer SP/RM/QC/5.10 200 ml 100 ml For 2 weeks Daily
SP-02
RO Water Tank,
3. Refer SP/RM/QC/5.10 200 ml 100 ml For 2 weeks Daily
SP-03
DM Water Plant,
4. Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
SP-04
DM Water Tank,
5. Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
SP-05
WFI Water, SP-
6. Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
06A
WFI Storage
7. Tank Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
SP-07
User Point-I, SP-
8. Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
08
User point-II,
9. Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
SP-09
Return WFI
10. Distribution Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
loop SP-10
Remarks: For location of Sampling points (SP) follow the Table No.-01.

7.4.2 SAMPLING SCHEDULE FOR PHASE - 2 VALIDATION:

Sample Quantity
S. Sampling Test to be Frequen
Duration
No. Point No. conducted Chemic Microbiologica cy
al l
Raw Water, SP-
1. Refer SP/RM/QC/5.10 200 ml 100 ml For 2 weeks Daily
01
RO Water Plant,
2. Refer SP/RM/QC/5.10 200 ml 100 ml For 2 weeks Daily
SP-02
3. RO Water Tank, Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
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Sample Quantity
S. Sampling Test to be Frequen
Duration
No. Point No. conducted Chemic Microbiologica cy
al l
SP-03
DM Water Plant,
4. Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
SP-04
DM Water Tank,
5. Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
SP-05
WFI Water, SP-
6. Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
06A
WFI Storage
7. Tank Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
SP-07
User Point-I, SP-
8. Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
08
User point-II,
9. Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
SP-09
Return WFI
10. Distribution Refer SP/RM/QC/5.11 500 ml 200 ml For 2 weeks Daily
loop SP-10

7.4.3 SAMPLING SCHEDULE FOR PHASE 3 OF VALIDATION:

Sample Quantity
S. Sampling Point Test to be Frequenc
Duration
No. No. conducted Chemic y
Microbiological
al
Refer For One
1. Raw Water, SP-01 200 ml 100 ml For
SP/RM/QC/5.10 Year
RO Water Plant, Refer For One chemical
2. 200 ml 100 ml testing &
SP-02 SP/RM/QC/5.10 Year
RO Water Tank, Refer For One Microbial
3. 500 ml 200 ml testing At
SP-03 SP/RM/QC/5.11 Year
least
DM Water Plant, Refer For One
4. 500 ml 200 ml weekly &
SP-04 SP/RM/QC/5.11 Year
so that all
DM Water Tank, Refer For One
5. 500 ml 200 ml sampling
SP-05 SP/RM/QC/5.11 Year
points
Refer For One
6. WFI Water, SP-06A 500 ml 200 ml must be
SP/RM/QC/5.11 Year
covered in
WFI Storage Tank Refer For One
7. 500 ml 200 ml a week.
SP-07 SP/RM/QC/5.11 Year
Pathogen
User Point-I, SP- Refer For One testing will
8. 500 ml 200 ml
08 SP/RM/QC/5.11 Year be
User point-II, SP- Refer For One conducted
9. 500 ml 200 ml
09 SP/RM/QC/5.11 Year every 15
Return WFI working
Refer For One
10. Distribution loop 500 ml 200 ml days.
SP/RM/QC/5.11 Year
SP-10
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8.0 MONITORING & CONTROLLING OF WATER SYSTEM

Describe the monitoring & controlling of water system. List the instruments / consumable
materials not installed on or part of the equipment and/or system being qualified that are
required for execution of this protocol. Document the identification of these materials, and the
calibration or expiration dates, if applicable.

Tota
Name of UO Calibratio
Location l Description/Purpose Due Date
Instruments M n Date
Qty.

Verified by (QA) Date

Criteria Met?
Acceptance Criteria
(Yes/No)
Are instruments calibrated and calibration certificates reviewed for
acceptance?

Remarks/
Comments
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9.0 TRAINING PROGRAM FOR PERSONNEL PERFORMING WATER SYSTEM VALIDATION

Name of the identified persons will perform the water system validation as under:

TRAINING GIVEN BY

Name

Designation

Signature/ Date

TRAINING TO EXECUTION TEAM

Name Designation Department Signature Date

Venue

Date of training

Duration of training
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10.0 ACCEPTANCE CRITERIA

10.1 SPECIFICATION FOR RAW WATER

S.No. Name of the tests Limit References

1 Description Clear and colorless liquid

2 pH Between 7.0 to 8.0

SP/RM/QC/5.10, Rev.
3 Hardness NMT 500 ppm
No.-01
4 Total microbial count NMT 500 CFU/ml

5 Pathogen test Should be absent

10.2 SPECIFICATION FOR R.O WATER

S.No. Name of the tests Limit References

1 Description Clear and colorless liquid

2 pH Between 6.5 to 8.5

3 Hardness NMT 1 ppm SP/RM/QC/5.10, Rev.

No.-01
4 Total Dissolve Solids (TDS) NMT 500 ppm

5 Total microbial count NMT 500 CFU/ml

6 Pathogen test Should be absent

10.3 SPECIFICATION FOR PURIFIED WATER

S. No. Test Specification References

1 Description Should be clear and colorless liquid

2 Conductivity NMT 1.3µmho

3 Oxidisable substances Should comply

4 Heavy Metals NMT 0.1 ppm

SP/RM/QC/5.11, Rev.
5 Nitrates NMT 0.2 ppm
No.-00
6 Acidity or Alkalinity Should comply

7 Total organic Carbon NMT 0.5 ppm

8 Total microbial count NMT 100 CFU/ml

9 Pathogen test Should be absent

10.4 SPECIFICATION FOR WATER FOR INJECTION

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S. No. Test Specification References

1 Description Should be clear and colorless liquid
2 Conductivity NMT 1.3µmho
3 Total organic Carbon NMT 0.5 ppm
4 Acidity or Alkalinity Should comply SP/RM/QC/5.11, Rev.
5 Nitrates NMT 0.2 ppm No.-00

6 Total microbial count NMT 10 CFU/ 100ml

7 Pathogen test Should be absent
8 Bacterial Endotoxin test NMT 0.25 E.U per ml

 IN CASE OF FAILURE MODE

Incase the water fails to meet the acceptance criteria during any phase of
validation, corrective and preventive action must be taken immediately.

11.0 DATA RECORDING

11.1 FOR CHEMICAL ANALYSIS: Raw water, RO water shall be recorded in

format F/QA/5.04, Rev.01

11.2 For Chemical analysis: Purified water and Water for injection shall be
recorded in format F/QA/5.05, Rev.00

11.3 FOR MICROBIOLOGICAL ANALYSIS:

Annex-01

Bio Burden (By Pour Plate Method) and Pathogen Test

Media Bio Pathogen Test

Date of
S. Date of Sterilizati Incubatio Sampling burden Done
Completio
No. Testing on Load n Temp. Points (CFU/ml S. P. By
n E. S.
No. ) aureu aerugino
coli enterica
s sa

SP-01

SP-02

SP-03

SP-04

SP-05

SP-01
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Bio Burden (By Pour Plate Method) and Pathogen Test

Media Bio Pathogen Test

Date of
S. Date of Sterilizati Incubatio Sampling burden Done
Completio
No. Testing on Load n Temp. Points (CFU/ml S. P. By
n E. S.
No. ) aureu aerugino
coli enterica
s sa

SP-02

SP-03

SP-04

SP-05

SP-01

SP-02

SP-03

SP-04

SP-05

Conclusion-: The above data shows that Raw water/ RO Water/ Purified water result comply/does not
comply as per specification mention in protocol.
Annex-02

Bio Burden (By Membrane Filtration Method) and Pathogen Test For WFI

Bio
burden Pathogen Test
Media
Date of Result
S. Date of Sterilizati Incubatio Sampling Done
Completio (Limit
No. Testing on Load n Temp. Points S. P. By
n 10 E. S.
No. aureu aerugino
CFU/10 coli enterica
s sa
0 ml)

SP-06A

SP-07

SP-08

SP-09

SP-10

SP-06A
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Bio Burden (By Membrane Filtration Method) and Pathogen Test For WFI

Bio
burden Pathogen Test
Media
Date of Result
S. Date of Sterilizati Incubatio Sampling Done
Completio (Limit
No. Testing on Load n Temp. Points S. P. By
n 10 E. S.
No. aureu aerugino
CFU/10 coli enterica
s sa
0 ml)

SP-07

SP-08

SP-09

SP-10

SP-06A

SP-07

SP-08

SP-09

SP-10

Conclusion-: The above data shows that WFI results comply/does not comply as per specification
mention in protocol.

11.4 BACTERIAL ENDOTOXIN TEST

Bacterial Endotoxin test shall be recorded in F/QA/5.49.

12.0 DEVIATION REPORT

Any deviation from the acceptance criteria of the specific check point shall be documented
in (F/QA/5.168, Rev.:-00) and decision should be taken for the rejection, replacement or
rectification of the machine/component.

13.0 WATER SYSTEM VALIDATION REPORT

The Water system validation reports should contain but not limited to the following -

 Title - the process or item that was evaluated.

 Purpose & Scope - as described above.
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WATER SYSTEM VALIDATION PROTOCOL
Document No. Revision No. 00
Effective date

 Reference Documents - Only if not included in the Protocol Plan.

 Results - The results of the testing.
 Deviations - Identify all deviations from the plan, with justification for the
changes.
 Conclusion - A summary of the results and a statement as to the “success” or
“failure” of the protocol.
 Raw Data - Raw data should be filed with the test report.

14.0 EVALUATION

The water system will be test during phase-1, phase-2 and phase 3 for its efficiency of
manufacturing, storage and distribution of WFI.

Evaluate all completed, signed data record forms. Completed summary data recorded in
form as per annexure– 1. Compare to acceptance criteria. Prepare Deviation Report
including the justification of acceptance and impact on the Performance as per point 8.0.
Prepare a Water system validation Report.

15.0 CONCLUSION

Based on the above results, it is concluded that the Water system validation of water
system will be complete as per operating procedure and testing reports and then released
for regular production.

16.0 REQUALIFICATION

Water System to be re-qualified on: -

 Replacement of major component with a new component.

 Any major modification in the existing equipment.

 Shifting of the equipment from one location to another.

 Any change in specification and regulatory requirements.