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PROTOCOL NO: QUALITY ASSURANCE DEPTT
BATCH NO. PAGE NO:- 1 0F 25
FORMULATION :
PRODUCT NAME :
LINE :
REASON FOR PERFORMING THE VALIDATION STUDY :
Reason ( tick which ever is applicable) Remarks
Department
New product
Modification in the manufacturing process.
Change in Facility and / or location of manufacturing.
Batch fail to meet product & process specifications.
Number of batches studied: ________________
Batch numbers: 1. _______________
2.. _______________
3. _______________
Validation activity authorized By: _____________________________Date:_______________________
Validation Team:
DEPARTMENT VALIDATION TEAM
PRODUCTION
QUALITY ASSURANCE
QUALITY CONTROL
REMARKS:
APPROVALS:
DEPARTMENT SIGN & DATE
PRODUCTION
QUALITY ASSUARANCE
QUALITY CONTROL
PRODUCT DEVLOPMENT
ENGINEERING
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1.1 GENERAL:
1.2 INTRODUCTION:
The process validation will be performed as prospective validation . The complete documentation for the
validation comprises several independent documents, references to relevant documents will be given as
part of this protocol, (see below). The results of the validation activities will be summarized in the
validation report.
1.3 LIST OF DOCUMENTS FOR VALIDATION:
Validation protocol,
Details of sampling for the validation batches, test parameters ( Product performance characteristics)
with reference to test methods & Acceptance criteria. (acceptable Limit)
Methods for recording / evaluating results including statistical analysis.
Reference to relevant documents.
1.2.2 BATCH MANUFACTURING RECORDS.
Detailed manufacturing instructions for the production of the validation batches.
2.0 PERSSONEL RESPONSIBILITIES.
SR ACTIVITY RESPONSIBILITY REMARKS
1 Preparation of validation protocol
2 Approval of Validation protocol
3 Production of validation Batches
4 Testing of validation samples &
Preparation of validation report
5 Approval of validation report.
3.0 PROCESS DESCIRPTION / FLOW SHEET
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The information given below provides a general description of the process. Detailed information for the
manufacturing will be supplied separately in the batch manufacturing record.
1.0 DISPENSING OF MATERIAL
2.0 WATER PHASE PREPARATION
3.0 GELATIN PREPARATION
4.0 MIXING
5.0 Q.C APPROVAL
6.0 FILLING , CRIMPING & CODING.
7.0 PACKING
3.1 FORMULATION:
BATCH SIZE:
SR Ingredients/excipients Specification Label Per Qnty of Total
claim batch overages
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
NOTE:
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3.2 FLOW SHEET:
DISPENSING OF MATERIAL
1. ADDITIONAL
QUALITY OF
WATER PHASE GELATIN PHASE 1. MIXING TIME
PURIFIED WATER ____ MINS./ SLOW 2. SPEED( RPM)
WATER ADDED. HEAT
2. TEMP. 3. TEMP.
3. SPEED( RPM)
____ MINS./ SLOW
Addition Of Addition Of
Excipient Active
Ingredient
Mixing
With Addition Of Active
Ingredient
____ Mins./ Slow 1. MIXING TIME
2. SPEED( RPM)
3. TEMP.
Q.C APPROVAL
1.0 WEIGHT / TUBE
2.0 CRIPING
3.0 CODING FILLING , CRIPING &
CODING
FINAL PACKING
4.0 EQUIPMENT / FACTORY.
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A detailed list of equipment used for validation together with the cleaning status will be provided in
the manufacturing documents.
4.1 LIST OF SOP’S , VALIDATION & QUALIFICATION REPORT USED AS REFERENCES
S ID. NUMBER TITLE VERIFIED DATE
R BY
1. Equipment cleaning procedure for Octagonal Steam
Jacketed Tank 350 ltr with stirrer ( for gelatin Phase)
2. Equipment Operating procedure for Octagonal Steam
Jacketed Tank 350 ltr with stirrer ( for gelatin Phase)
3. Equipment operating procedure for 500 ltr.
manufacturing tank with Homonizer and anchor stirrer.
4. Equipment cleaning procedure for 500 ltr manufacturing
tank with Homonizer and anchor stirrer.
5. Equipment cleaning procedure for storage tank.
6. Equipment operating procedure for storage tank
7. Equipment cleaning procedure for Capsule filling
machine
8. Equipment operating procedure for Capsule filling
machine
9. Enter any other reference sop.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
4.2 DETAILS OF EQUIPMENT TO BE USED.
EQUIPMENT DETAILS
BALANCE TYPE :
MODEL:
CAPACITY:
MANUACTURER:
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BATCH NO. PAGE NO:- 6 0F 25
[Link].:
M.O.C.
WATER PHASE TYPE :
[Link] MODEL:
CAPACITY:
MANUACTURER:
[Link].:
M.O.C.
GELATIN TANK : TYPE :
MODEL:
CAPACITY:
MANUACTURER:
[Link].:
M.O.C.
MFG. TANK : TYPE :
MODEL:
CAPACITY:
MANUACTURER:
[Link].:
M.O.C.
EQUIPMENT DETAILS
STORAGE TANK: TYPE :
MODEL:
CAPACITY:
MANUACTURER:
[Link].:
M.O.C.
CAPSULE FILLING TYPE :
MACHINE: MODEL:
CAPACITY:
MANUACTURER:
[Link].:
M.O.C.
TRANSFER PUMP: TYPE :
MODEL:
CAPACITY:
MANUACTURER:
[Link].:
M.O.C.
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REMARKS:
4.3 IDENTIFICATION OF CRITICAL PROCESS VARIABLES/ PARAMETER.
4.3.1 PROBABLE CAUSES THAT MAY EFFECT FINAL PRODUCT:
DISPENSING OF OIL PHASE SOLUTION TUBE FILLING
MATERIAL PREPARATION
LOAD SIZE SPEED
ACTIVE
SPEED
TEMPERATURE WEIGHT/TUBE
EXCIPIENT
PH
TEMPERATURE
COOLING
TEMPERATURE
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SPEED
LOAD SIZE Checked by Approved
SPEED by
BOILING LOAD SIZE
TEMPERATURE
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CRITICAL PROCESS PARAMETERS:
SR CRITICAL PRECESS RESPONSE PARAMETER REMARKS
VERIABLE
1 WATER PHASE SOLUTION
PREPARATION
Sequence of excipient addition Water phase uniformity Fixed order of addition
Water Boiling Temperature Fixed Boiling temperature range
Time Variation of time for boiling
Heating Temperature Fixed Heating temperature range
Time Variation of time for heating
Cooling Temperature Fixed cooling temperature range
Time Variation of time for cooling
PH Fixed limit of Ph
Mixing time Variation of mixing time (RPM)
2 GELATIN PREPARATION
Sequence of excipient addition Fixed order of addition
Heating Temperature GELATIN uniformity Fixed Heating temperature range
Time Variation of time for heating
Cooling Temperature Fixed cooling temperature range
Time Variation of time for cooling
Mixing time Variation of mixing time (RPM)
3 MANUFACTURING
Sequence of Active addition Fixed order of addition
Mixing time Active ingredient uniformity Variation of mixing time
Cooling Temperature Fixed temperature range
4 Filling, Crimping & Coding
Filling speed 1. Weight of tube Fixed machine speed, no
2. Crimping variation.
CRITICAL PROCESS VARIABLE:
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SR PROCESS / VARIABLE MACHINE SETTING REMARKS
(CONTROL VARIABLES)
1 Water Phase Solution Quantity of water
Preparation Setting and conditions as mentioned
2 GELATIN Preparation Quantity of paraffin & wax
in the batch manufacturing record to
& other CONSTITUENTS.
3 Manufacturing Mixing time be followed.
Cooling Time
4 Filling Speed, weight / tube.
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5.0 SAMPLING , TEST PARAMETERS, ACCEPTANCE CIRTERIA
5.1 Sampling Locations:
Mfg. Tank.
1. TOP –SAMPLE A1
2. MIDDLE –SAMPLE A2
3. BOTTAM –SAMPLE A3
BOTTOM VALVE
5.3 SAMPLING
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STAGE/ TEST PARAMETER SAMPLING REMARKS
( SIZE,LOCATION,TIME)
Water phase solution preparation After the completion of water Record amount of water ,
phase solution , Temperature & time required to
N=1 sample ( pooled from achieve desired end point/
different locations) ampere reading.
Sample size =20 gm
Oil phase solution preparation After the completion of Oil phase Record amount of oil,
solution , Temperature & time required to
N=1 sample ( pooled from achieve desired end point/
different locations) ampere reading.
Sample size =20 gm
MANUFACTURING After 20 min of mixing time, Record the pH and assay of
After 30 minutes & after 40
active content .
PH,
minutes.
N=3 samples at each interval
ASSAY
Sample size: 20 gm
Filling Draw the sample entire filling Each sample comprises the
assembly, consisting of transfer amount for the different tests
pump & holding tank and filling required.
Identification test machine.
Appearance Sample draw from each
Uniformity of Weight syringes as a set weight at
Assay of active content. different time interval.
Sampling : at start, every two
hours, immediately after the
brake time , end of filling..
Sample size :__________.
STAGE / TEST PARAMETER EQUIPMENT ACCEPTANCE CRITERIA
( SIZE , LOCATION, TIME)
Water phase solution preparation Determination on each sample, 80 + 50C
for temperature, sample weight
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10 g.
Oil phase solution preparation Determination on each sample, 80 + 50C
for temperature, sample weight
10 g.
Manufacturing Sampling thief: Assay 90 % to 110 %
ASSAY Rel. std. :
PH
FILLING
Appearance Visual inspection, As specified in the BMR.
Weight of Tubes. Analytical balance _____ gm (_____gm - _____ gm)
Weight variation Analytical balance _______ % of average weight.
Identification test H.P.L.C. Test should complies to its
specifications.
90 % to 110 %
Assay:
6.0 RECORDING OF DATA & DATA TREATMENT
6.1DATA RECORDING
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BATCH NO. PAGE NO:- 13 0F 25
The data obtained from the various analysis & observations shall be recorded in the DATA
RECORDING SHEET for first three commercial batches.
DATA RECORDING
SHEET NO.
SHEET NO 1 For recording water phase mixing observation & results
SHEET NO 2 For recording oil phase mixing observations & results.
SHEET NO 3 For recording Bulk manufacturing observations & results.
SHEET NO 4 For recording assay results after filling and crimping operation.
SHEET NO 5 For recording general utilities /equipment / method Analytical /results.
SHEET NO 6 For recording analytical method validation.
SHEET NO 7
SHEET NO 8
SHEET NO 9
SHEET NO 10
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DATA RECORDING SHEET #1
WATER PHASE SOLUTION PREPARATION
Equipment Name :_________________________
Identification no :_________________________ Date:___________________
Capacity : ______________________lt.
Ingredients and sequence of material addition: ____________________
Total weight of ingredients : _______________kg/lot.
Mixing time : 20 minutes
Setting – stirrer : slow
Procedure : As outlined in the batch manufacturing record.
Plan : Samples to be drawn at of 20 minutes, 30 minutes, & 40 minutes of mixing
from 3 different locations
FOR WATER PHASE SOLUTION TANK-RESULTS. BATCH NO:
Assay of after mixing AT 20 MIN..
RESULTES
Sample no: Temperature Uniformity
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL
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Assay of after mixing AT 30 MIN..
RESULTES
Sample no: Temperature Uniformity
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL
Assay of after mixing AT 40 MIN..
RESULTES
Sample no: Temperature Uniformity
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL
Actual Temperature of the water/binder : ___________ 0C
Temperature of the water after heating : ___________ 0C
Temperature of the water after cooling : ___________ 0C
Additional quantity of water added (ltr.):____________
Total time taken : ___________
POINTS
Method of analysis adopted
Ref No.:
Analyst:
Date
Meet acceptance criteria. YES ( ) NO ( )
CONCLUSIONS:________________________________________________________________________
_______________________________________________________________________________________
_______________________________________________________________________________________
CHECKED BY:_________________________ DATE____________________
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DATA RECORDING SHEET # 2
OIL PHASE SOLUTION PREPARATION
Equipment Name :_________________________
Identification no :_________________________ Date:___________________
Capacity : ______________________lt.
Ingredients and sequence of material addition: ____________________
Total weight of ingredients : _______________kg/lot.
Mixing time : 20 minutes
Setting – stirrer : slow
Procedure : As outlined in the batch manufacturing record.
Plan : Samples to be drawn at of 20 minutes, 30 minutes, & 40 minutes of mixing from
3 different locations
FOR OIL PHASE SOLUTION TANK-RESULTS. BATCH NO:
Assay of after mixing AT 20 MIN..
RESULTES
Sample no: Temperature Uniformity
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL
Assay of after mixing AT 30 MIN..
RESULTES
Sample no: Temperature Uniformity
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL
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Assay of after mixing AT 40 MIN..
RESULTES
Sample no: Temperature Uniformity
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL
Actual Temperature of the water/binder : ___________0C
Temperature of the water after heating : ___________0C
Temperature of the water after cooling : ___________0C
Additional quantity of water added (ltr.):____________
Total time taken : ___________
POINTS
Method of analysis adopted
Ref No.:
Analyst:
Date
Meet acceptance criteria. YES ( ) NO ( )
CONCLUSIONS:________________________________________________________________________
_______________________________________________________________________________________
_______________________________________________________________________________________
CHECKED BY:_________________________ DATE____________________
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DATA RECORDING SHEET # 3
MANUFACTURING :
Equipment Name :_________________________
Identification no :_________________________ Date:___________________
Capacity : ______________________lt.
Ingredients and sequence of material addition: ____________________
Total weight of ingredients : _______________kg/lot.
Mixing time : 20 minutes
Setting – stirrer : slow
Procedure : As outlined in the batch manufacturing record.
Plan : Samples to be drawn at of 20 minutes, 30 minutes, & 40 minutes of mixing
from 3 different locations
FOR MANUFCTURING TANK-RESULTS. BATCH NO:
Assay of after mixing AT 20 MIN..
Sample no: PH ASSAY REMARK
1
2
3
Average std. Dev.
Range
RSD
LCL
UCL
Assay of after mixing AT 30 MIN..
Sample no: PH ASSAY REMARK
1
2
3
Average std. Dev.
Range
RSD
LCL
UCL
Assay of after mixing AT 40 MIN..
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Sample no: PH ASSAY REMARK
1
2
3
Average std. Dev.
Range
RSD
LCL
UCL
POINTS
Method of analysis adopted
Ref No.:
Analyst:
Date
Meet acceptance criteria. YES ( ) NO ( )
CONCLUSIONS:________________________________________________________________________
_______________________________________________________________________________________
_______________________________________________________________________________________
CHECKED BY:_________________________ DATE____________________
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DATA RECORDING SHEET # 4
FILLING & CRIMPING :
Equipment Name :_________________________
Identification no :_________________________ Date:___________________
Capacity : ______________________lt.
Mixing time( filling hopper) : Continues stirring during filling
Setting – stirrer : slow ( R.P.M._________)
Procedure : As outlined in the batch manufacturing record.
Plan : Samples to be drawn from each syringes as set weight at different time
interval as mention below:
1. Initional ( 0 time)
2. Every 2 hours
3. Immediately after the break time
4. At the end of filling
from 3 different locations
FOR FILLING MACHINE -RESULTS. BATCH NO:
SAMPLE NO: APPEARANCE WEIGHT IDENTIFICATIO ASSAY
N TEST
Initional ( 0 time)
Every 2 hours
Immediately after the
break time
At the end of filling
Average std. Dev.
Range
RSD
LCL
UCL
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Assay of after mixing AT 30 MIN..
SAMPLE NO: APPEARANCE WEIGHT IDENTIFICATION TEST ASSAY
Initional ( 0 time)
Every 2 hours
Immediately after the
break time
At the end of filling
Average std. Dev.
Range
RSD
LCL
UCL
Assay of after mixing AT 40 MIN..
SAMPLE NO: APPEARANCE WEIGHT IDENTIFICATION TEST ASSAY
Initional ( 0 time)
Every 2 hours
Immediately after the
break time
At the end of filling
Average std. Dev.
Range
RSD
LCL
UCL
POINTS
Method of analysis adopted
Ref No.:
Analyst:
Date
Meet acceptance criteria. YES ( ) NO ( )
CONCLUSIONS:________________________________________________________________________
_______________________________________________________________________________________
_______________________________________________________________________________________
CHECKED BY:_________________________ DATE____________________
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DATA RECORDING SHEET # 5
DATE:____________________
SR NAME OF CRITICAL EQUIPMENT/UTILITIES QUALIFICATION/ DATE OF
VALIDATION FILE QUALIFICATION /
[Link]. VALIDATION
1 S.S 350 Octagonal Steam Jacketed Tank.
2 S.S 350 Octagonal Steam Jacketed Tank.
( OIL PHASE)
3 500 Octagonal Steam Jacketed Tank
4 Storage Vessel
6 Filling ,crimping & Coding machine
UTILITIES:
1 AHU SYSTEM
2 WATER SYSTEM
3 COMPRESSED AIR
4 STEAM
5 LIGHTNING
6 DRAIN
DATA RECORDING SHEET # 6
DATE:____________________
NAME OF PRODUCT:
SR Parameters Type of Actual Observed Analysis Analysis Ref.
sample reading reading performed checked by Work
by sheet
1 Accuracy Sample A
% Recovery of (known
known amount. amount of
analysis.
90 % of A
110 % of A
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2 Precision Sample A1
Repeatability ( from one
( under same sample
condition ) Test point)
by same analyst Sample A2
at same time ( from
from same second
homogenous sample
validated mass point)
but from Sample A3
different sample ( from third
plan ( by taking sample
sample of point)
different
quantity)
3 Reproducibility Sample A1
under different On ______
conditions.
Sample A2
On ______
Test by
different analyst Sample A3
on different On ______
days.
SR Parameters Type of Actual Observed Analysis Analysis Ref. Work
sample reading reading performe checked sheet
d by by
4 Linearity and range 25 % of A
Response 50 % of A
concentration curve 75 % of A
on graph paper. 100 % of A
125 % of A
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5 Specificity/ Sample A1
selectivity( by 15 min.
larger degradation
communication of
analytical method.)
for identification of
impurities assay of
active component Sample A2
etc…Temp & 30 min.
humidity / degradation
degradation
factored to main
ingredients by 15
min, 30 min,45 min
of heating or Sample A3
known degraded 45 min.
products. degradation
6 Limit of detection 1.1 % of A
( LOD) & limit of
quantitative (LOQ) 1% of A
Qualitative &
Quantitative result 5 % of A
10 % of A
20 % of A
7 Analysis method Method A
(for non
pharmacopoeial to Method B
be performed by
other public lab. Method C
REMARKS:
1. Specifically / selectivity analysis(4) and Reproducibility (2B) also given raggedness and robustness.
2. Limit of Quantitative (5) also gives sensitivity of test procedure.
Above procedure to be repeated over three batches to get minimum nine variables for each parameter.
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