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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 1 2 3 4
ACTIVITY Preparation of validation protocol Approval of Validation protocol Production of validation Batches Testing of validation samples &
5
Preparation of validation report Approval of validation report.
RESPONSIBILITY
REMARKS
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
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
ADDITIONAL QUALITY OF WATER ADDED. TEMP. SPEED( RPM) MIXING TIME
WATER PHASE PURIFIED WATER
HEAT
OIL PHASE ____ MINS./ SLOW
____ MINS./ SLOW
Addition Of Excipient
1. MIXING TIME 2. SPEED( RPM) 3. TEMP.
Addition Of Active Ingredient
Mixing With Addition Of Active Ingredient ____ Mins./ Slow
1. MIXING TIME 2. SPEED( RPM) 3. TEMP.
Q.C APPROVAL WEIGHT / TUBE CRIPING 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 SR
ID. NUMBER
1.
TITLE
VERIFIED BY
Equipment cleaning procedure for Octagonal Steam Jacketed Tank 350 ltr with stirrer ( for Oily Phase) Equipment Operating procedure for Octagonal Steam Jacketed Tank 350 ltr with stirrer ( for Oily Phase) Equipment operating procedure for 500 ltr. manufacturing tank with Homonizer and anchor stirrer. Equipment cleaning procedure for 500 ltr manufacturing tank with Homonizer and anchor stirrer. Equipment cleaning procedure for storage tank. Equipment operating procedure for storage tank Equipment cleaning procedure for Tube filling machine Equipment operating procedure for Tube filling machine Enter any other reference sop.
2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.
4.2 DETAILS OF EQUIPMENT TO BE USED. EQUIPMENT BALANCE
DETAILS TYPE : MODEL: CAPACITY: MANUACTURER: TAG.NO.: M.O.C. TYPE : Approved by
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DATE
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WATER PHASE S.S.TANK
OIL PHASE TANK :
MFG. TANK :
EQUIPMENT STORAGE TANK:
TUBE FILLING MACHINE:
TRANSFER PUMP:
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MODEL: CAPACITY: MANUACTURER: TAG.NO.: M.O.C. TYPE : MODEL: CAPACITY: MANUACTURER: TAG.NO.: M.O.C. TYPE : MODEL: CAPACITY: MANUACTURER: TAG.NO.: M.O.C.
DETAILS TYPE : MODEL: CAPACITY: MANUACTURER: TAG.NO.: M.O.C. TYPE : MODEL: CAPACITY: MANUACTURER: TAG.NO.: M.O.C. TYPE : MODEL: CAPACITY: MANUACTURER: TAG.NO.: M.O.C.
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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
LOAD SIZE
SPEED
ACTIVE
SPEED
WEIGHT/TUBE
TEMPERATURE EXCIPIENT
PH
TEMPERATURE
COOLING TEMPERATURE
SPEED
SPEED
LOAD SIZE BOILING TEMPERATURE Prepared by WATER PHASE SOLUTION PREPARATION
LOAD SIZE
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CRITICAL PROCESS PARAMETERS: SR 1
2
3
4
CRITICAL PRECESS VERIABLE WATER PHASE SOLUTION PREPARATION Sequence of excipient addition Water Boiling Temperature Time Heating Temperature Time Cooling Temperature Time PH Mixing time OIL PHASE SOLUTION PREPARATION Sequence of excipient addition Heating Temperature Time Cooling Temperature Time Mixing time MANUFACTURING Sequence of Active addition Mixing time Cooling Temperature Filling, Crimping & Coding Filling speed
RESPONSE PARAMETER
REMARKS
Water phase uniformity
Fixed order of addition Fixed Boiling temperature range Variation of time for boiling Fixed Heating temperature range Variation of time for heating Fixed cooling temperature range Variation of time for cooling Fixed limit of Ph Variation of mixing time (RPM)
Oil phase uniformity Fixed order of addition Fixed Heating temperature range Variation of time for heating Fixed cooling temperature range Variation of time for cooling Variation of mixing time (RPM) Active ingredient uniformity
1. Weight of tube 2. Crimping
Fixed order of addition Variation of mixing time Fixed temperature range Fixed machine speed, no variation.
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CRITICAL PROCESS VARIABLE: SR
PROCESS / VARIABLE
MACHINE SETTING
1
Water Phase Solution
(CONTROL VARIABLES) Quantity of water
2
Preparation Oil Phase Solution
Quantity of paraffin & wax
3
Preparation Manufacturing
& other oil. Mixing time
4
Filling
Cooling Time Speed, weight / tube.
REMARKS
Setting and conditions as mentioned in the batch manufacturing record to be followed.
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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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STAGE/ TEST PARAMETER Water phase solution preparation
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SAMPLING ( SIZE,LOCATION,TIME) After the completion of water
Record amount of water ,
phase solution ,
Temperature & time required to
N=1 sample ( pooled from
achieve desired end point/ ampere
different locations) Oil phase solution preparation
PH, ASSAY
Filling
reading.
Sample size =20 gm After the completion of Oil phase
Record amount of oil,
solution ,
Temperature & time required to
N=1 sample ( pooled from
achieve desired end point/ ampere
different locations) MANUFACTURING
REMARKS
Sample size =20 gm After 20 min of mixing time, After 30 minutes & after 40 minutes. N=3 samples at each interval Sample size: 20 gm Draw the sample entire filling
reading. Record the pH and assay of active content .
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 ( SIZE , LOCATION, TIME)
ACCEPTANCE CRITERIA
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Water phase solution preparation Oil phase solution preparation Manufacturing
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Determination on each sample, for
80 + 50C
temperature, sample weight 10 g. Determination on each sample, for temperature, sample weight 10 g. Sampling thief:
80 + 50C
ASSAY
Assay 90 % to 110 % 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
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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 SHEET NO 2 SHEET NO 3 SHEET NO 4 SHEET NO 5 SHEET NO 6 SHEET NO 7 SHEET NO 8 SHEET NO 9 SHEET NO 10
For recording water phase mixing observation & results For recording oil phase mixing observations & results. For recording Bulk manufacturing observations & results. For recording assay results after filling and crimping operation. For recording general utilities /equipment / method Analytical /results. For recording analytical method validation.
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DATA RECORDING SHEET #1 WATER PHASE SOLUTION PREPARATION Equipment Name
:_________________________
Identification no
:_________________________
Capacity
: ______________________lt.
Date:___________________
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.. Sample no: 1 2 3 Average std. Dev. Range RSD LCL UCL
Temperature
RESULTES Uniformity
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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____________________ Approved by
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DATA RECORDING SHEET # 2 OIL PHASE SOLUTION PREPARATION Equipment Name
:_________________________
Identification no
:_________________________
Capacity
: ______________________lt.
Date:___________________
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 from 3 different locations
: Samples to be drawn at of 20 minutes, 30 minutes, & 40 minutes of mixing
FOR OIL PHASE SOLUTION TANK-RESULTS. Assay of after mixing AT 20 MIN.. Sample no: 1 2 3 Average std. Dev. Range RSD LCL UCL
Temperature
BATCH NO:
RESULTES Uniformity
Assay of after mixing AT 30 MIN.. RESULTES Sample no: Temperature Uniformity 1 2 3 Average std. Dev. Range RSD LCL UCL Approved by Prepared by
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Assay of after mixing AT 40 MIN.. Sample no: 1 2 3 Average std. Dev. Range RSD LCL UCL
Temperature
RESULTES Uniformity
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
:_________________________
Capacity
: ______________________lt.
Date:___________________
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. Assay of after mixing AT 20 MIN.. Sample no: 1 2 3 Average std. Dev. Range RSD LCL UCL
PH
Assay of after mixing AT 30 MIN.. Sample no: PH 1 2 3 Average std. Dev. Range RSD LCL UCL
BATCH NO:
ASSAY
REMARK
ASSAY
REMARK
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Assay of after mixing AT 40 MIN.. Sample no: 1 2 3 Average std. Dev. Range RSD LCL UCL
PH
ASSAY
REMARK
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
:_________________________
Capacity
: ______________________lt.
Date:___________________
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. SAMPLE NO:
APPEARANCE
BATCH NO: WEIGHT IDENTIFICATION ASSAY 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: Initional ( 0 time) Every 2 hours Immediately after the break time At the end of filling
APPEARANCE
WEIGHT IDENTIFICATION TEST
ASSAY
WEIGHT IDENTIFICATION TEST
ASSAY
Average std. Dev. Range RSD LCL UCL Assay of after mixing AT 40 MIN.. SAMPLE NO: Initional ( 0 time) Every 2 hours Immediately after the break time At the end of filling
APPEARANCE
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____________________ Approved by
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DATA RECORDING SHEET # 5 DATE:____________________ SR
NAME OF CRITICAL EQUIPMENT/UTILITIES
1 2
S.S 350 Octagonal Steam Jacketed Tank. S.S 350 Octagonal Steam Jacketed Tank.
3 4 6
( OIL PHASE) 500 Octagonal Steam Jacketed Tank Storage Vessel Filling ,crimping & Coding machine
QUALIFICATION/ VALIDATION FILE REF.NO.
DATE OF QUALIFICATION / VALIDATION
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 sample
1
Sample A (known amount of analysis.
Accuracy % Recovery of known amount.
Actual reading
Observed reading
Analysis performed by
Analysis checked by
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Ref. Work sheet
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2
3
QUALITY ASSURANCE DEPTT PAGE NO:- 23 0F 25
90 % of A 110 % of A 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) Reproducibility Sample A1 under different On ______ conditions. Sample A2 On ______ Test by different analyst Sample A3 on different On ______ days.
SR Parameters
Type of sample
4
25 % of A 50 % of A 75 % of A 100 % of A 125 % of A
Linearity and range Response concentration curve on graph paper.
Actual reading
Observed reading
Analysis Analysis performed checked by by
Ref. Work sheet
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5
6
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. Limit of detection ( LOD) & limit of quantitative (LOQ) Qualitative & Quantitative result
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Sample A1 15 min. degradation
Sample A2 30 min. degradation
Sample A3 45 min. degradation 0.1 % of A 1% of A 5 % of A 10 % of A
7
Analysis method (for non pharmacopoeial to be performed by other public lab.
20 % of A Method A Method B 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. Approved by Prepared by
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