Ointment Process Validation-Original
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Transcript of Ointment Process Validation-Original
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PROCESS VALIDATION PROTOCOL (OINTMENT)
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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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1.0 GENERAL:
1.1 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.
1.2 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 OIL PHASE 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 claim
Per batch
Qnty of overages
Total
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
WATER PHASE PURIFIED WATER
HEAT
____ MINS./ SLOW
OIL PHASE ____ MINS./ SLOW
Mixing With Addition Of Active
Ingredient ____ Mins./ Slow
FILLING , CRIPING & CODING
FINAL PACKING
1. ADDITIONAL QUALITY OF WATER ADDED.
2. TEMP. 3. SPEED( RPM)
1.0 WEIGHT / TUBE 2.0 CRIPING 3.0 CODING
1. MIXING TIME 2. SPEED( RPM) 3. TEMP.
1. MIXING TIME 2. SPEED( RPM) 3. TEMP.
Addition Of Active
Ingredient
Addition Of Excipient
Q.C APPROVAL
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4.0 EQUIPMENT / FACTORY.
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 SR ID. NUMBER TITLE VERIFIED
BY DATE
1. Equipment cleaning procedure for Octagonal Steam Jacketed Tank 350 ltr with stirrer ( for Oily Phase)
2. Equipment Operating procedure for Octagonal Steam Jacketed Tank 350 ltr with stirrer ( for Oily 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 Tube filling machine
8. Equipment operating procedure for Tube filling machine
9. Enter any other reference sop.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
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4.2 DETAILS OF EQUIPMENT TO BE USED.
EQUIPMENT DETAILS BALANCE TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
WATER PHASE S.S.TANK
TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
OIL PHASE TANK : TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
MFG. TANK : TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
EQUIPMENT DETAILS
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STORAGE TANK: TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
TUBE FILLING MACHINE:
TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
TRANSFER PUMP: TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
REMARKS:
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4.3 IDENTIFICATION OF CRITICAL PROCESS VARIABLES/ PARAMETER. 4.3.1 PROBABLE CAUSES THAT MAY EFFECT FINAL PRODUCT:
DISPENSING OF MATERIAL
OIL PHASE SOLUTION PREPARATION
TUBE FILLING
WATER PHASE SOLUTION PREPARATION
MANUFACTURING
EXCIPIENT
ACTIVE
LOAD SIZE
SPEED
TEMPERATURE
LOAD SIZE SPEED
COOLING TEMPERATURE
SPEED
LOAD SIZE
TEMPERATURE
PH
BOILING TEMPERATURE
SPEED
WEIGHT/TUBE
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CRITICAL PROCESS PARAMETERS: SR CRITICAL PRECESS
VERIABLE RESPONSE PARAMETER REMARKS
1 WATER PHASE SOLUTION PREPARATION
Water phase uniformity
Sequence of excipient addition 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 OIL PHASE SOLUTION
PREPARATION
Oil phase uniformity
Sequence of excipient addition Fixed order of addition Heating Temperature 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
Active ingredient uniformity
Sequence of Active addition Fixed order of addition Mixing time Variation of mixing time Cooling Temperature Fixed temperature range 4 Filling, Crimping & Coding
1. Weight of tube 2. Crimping
Filling speed Fixed machine speed, no
variation.
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CRITICAL PROCESS VARIABLE: SR PROCESS / VARIABLE MACHINE SETTING
(CONTROL VARIABLES)
REMARKS
1 Water Phase Solution
Preparation
Quantity of water
Setting and conditions as mentioned in
the batch manufacturing record to be
followed.
2 Oil Phase Solution
Preparation
Quantity of paraffin & wax
& other oil.
3 Manufacturing Mixing time
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
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5.3 SAMPLING STAGE/ TEST PARAMETER SAMPLING
( SIZE,LOCATION,TIME) REMARKS
Water phase solution preparation After the completion of water
phase solution ,
N=1 sample ( pooled from
different locations)
Sample size =20 gm
Record amount of water ,
Temperature & time required to
achieve desired end point/ ampere
reading.
Oil phase solution preparation After the completion of Oil phase
solution ,
N=1 sample ( pooled from
different locations)
Sample size =20 gm
Record amount of oil,
Temperature & time required to
achieve desired end point/ ampere
reading.
MANUFACTURING
PH,
ASSAY
After 20 min of mixing time, After 30 minutes & after 40 minutes. N=3 samples at each interval Sample size: 20 gm
Record the pH and assay of active
content .
Filling
Identification test
Appearance
Uniformity of Weight
Assay of active content.
Draw the sample entire filling
assembly, consisting of transfer
pump & holding tank and filling
machine.
Sample draw from each
syringes as a set weight at
different time interval.
Sampling : at start, every two
hours, immediately after the
brake time , end of filling..
Sample size :__________.
Each sample comprises the
amount for the different tests
required.
STAGE / TEST PARAMETER EQUIPMENT ACCEPTANCE CRITERIA
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( SIZE , LOCATION, TIME) Water phase solution preparation Determination on each sample, for
temperature, sample weight 10 g.
80 + 50C
Oil phase solution preparation Determination on each sample, for temperature, sample weight 10 g.
80 + 50C
Manufacturing
ASSAY
PH
Sampling thief: Assay 90 % to 110 %
Rel. std. :
FILLING
Appearance
Weight of Tubes.
Weight variation
Identification test
Assay:
Visual inspection,
Analytical balance
Analytical balance
H.P.L.C.
As specified in the BMR.
_____ gm (_____gm - _____ gm)
_______ % of average weight.
Test should complies to its
specifications.
90 % to 110 %
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6.0 RECORDING OF DATA & DATA TREATMENT
6.1DATA RECORDING
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
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Assay of after mixing AT 40 MIN.. 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 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
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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/
VALIDATION FILE REF.NO.
DATE OF QUALIFICATION / 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
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DATA RECORDING SHEET # 6 DATE:____________________ NAME OF PRODUCT: SR Parameters Type of
sample Actual reading
Observed reading
Analysis performed by
Analysis checked by
Ref. Work sheet
1 Accuracy % Recovery of known amount.
Sample A (known amount of analysis.
90 % of A 110 % of A
2 Precision Repeatability ( under same condition ) Test by same analyst at same time from same homogenous validated mass but from different sample plan ( by taking sample of different quantity)
Sample A1 ( from one sample point)
Sample A2 ( from second sample point)
Sample A3 ( from third sample point)
3 Reproducibility under different conditions. Test by different analyst on different days.
Sample A1 On ______
Sample A2 On ______
Sample A3 On ______
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SR Parameters Type of sample
Actual reading
Observed reading
Analysis performed by
Analysis checked by
Ref. Work sheet
4 Linearity and range Response concentration curve on graph paper.
25 % of A 50 % of A 75 % of A 100 % of A 125 % of A
5 Specificity/ selectivity( by larger communication of analytical method.) for identification of impurities assay of active component etc…Temp & humidity / degradation factored to main ingredients by 15 min, 30 min,45 min of heating or known degraded products.
Sample A1 15 min. degradation
Sample A2 30 min. degradation
Sample A3 45 min. degradation
6 Limit of detection ( LOD) & limit of quantitative (LOQ) Qualitative & Quantitative result
0.1 % of A
1% of A
5 % of A
10 % of A
20 % of A 7 Analysis method
(for non pharmacopoeial to be performed by other public lab.
Method A
Method B
Method C
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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.