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xxxxxxxxxxxxxxxxxxxxxxxxxxxx PROCESS VALIDATION PROTOCOL (OINTMENT

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 1 0F 26

FORMULATION

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PRODUCT NAME : LINE :

REASON FOR PERFORMING THE VALIDATION STUDY : Reason ( tick which ever is applicable) 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 PRODUCTION QUALITY ASSURANCE QUALITY CONTROL REMARKS: APPROVALS: DEPARTMENT PRODUCTION QUALITY ASSUARANCE QUALITY CONTROL PRODUCT DEVLOPMENT ENGINEERING SIGN & DATE VALIDATION TEAM Remarks

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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 1 Preparation of validation protocol 2 3 4 Approval of Validation protocol Production of validation Batches Testing of validation samples & Preparation of validation report 5 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 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 NOTE: Ingredients/excipients Specification Label claim Per batch Qnty of overages Total

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3.2 FLOW SHEET: DISPENSING OF MATERIAL

1.

2. 3.

ADDITIONAL QUALITY OF WATER ADDED. TEMP. SPEED( RPM)

WATER PHASE
PURIFIED WATER

HEAT

OIL PHASE ____ MINS./ SLOW

____ MINS./ SLOW

1. MIXING TIME 2. SPEED( RPM) 3. TEMP.

Addition Of Excipient

Addition Of 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

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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 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. ID. NUMBER TITLE 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. VERIFIED BY DATE

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4.2 DETAILS OF EQUIPMENT TO BE USED. EQUIPMENT BALANCE DETAILS 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

LOAD SIZE
ACTIVE

SPEED SPEED

TEMPERATURE

WEIGHT/TUBE

EXCIPIENT

PH

COOLING TEMPERATURE

TEMPERATURE

SPEED LOAD SIZE BOILING TEMPERATURE LOAD SIZE

SPEED

WATER PHASE SOLUTION PREPARATION

MANUFACTURING

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CRITICAL PROCESS PARAMETERS: SR 1 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)

2

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) Fixed order of addition Variation of mixing time Fixed temperature range Fixed machine speed, no variation.

3

Active ingredient uniformity

4

1. Weight of tube 2. Crimping

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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 Quantity of paraffin & wax & other oil. Mixing time Cooling Time the batch manufacturing record to be followed.

2

Oil Phase Solution Preparation

3

Manufacturing

4

Filling

Speed, weight / tube.

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 11 0F 26

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 Water phase solution preparation SAMPLING ( SIZE,LOCATION,TIME) After the completion of water phase solution ,  N=1 sample ( pooled from different locations)  Sample size =20 gm Oil phase solution preparation After the completion of Oil phase solution ,  N=1 sample ( pooled from different locations) Sample size =20 gm
MANUFACTURING

REMARKS Record amount of water , Temperature & time required to achieve desired end point/ ampere reading.

Record amount of oil, Temperature & time required to achieve desired end point/ ampere reading.

PH, ASSAY

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 assembly, consisting of transfer pump & holding tank and filling

Record the pH and assay of active content .

Filling

Each sample comprises the amount for the different tests required.

Identification test Appearance Uniformity of Weight Assay of active content.

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 :__________.

STAGE / TEST PARAMETER

EQUIPMENT

ACCEPTANCE CRITERIA

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Water phase solution preparation

( SIZE , LOCATION, TIME) Determination on each sample, for temperature, sample weight 10 g.

 80 + 50C  80 + 50C  Assay 90 % to 110 %  Rel. std. :

Oil phase solution preparation Manufacturing
ASSAY PH

Determination on each sample, for temperature, sample weight 10 g. Sampling thief:

FILLING Appearance Weight of Tubes. Weight variation Identification test 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 % Assay:

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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 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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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 15 0F 26

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 Mixing time Setting – stirrer Procedure Plan from 3 different locations FOR WATER PHASE SOLUTION TANK-RESULTS. BATCH NO: : _______________kg/lot. : 20 minutes : slow : As outlined in the batch manufacturing record. : Samples to be drawn at of 20 minutes, 30 minutes, & 40 minutes of mixing

Assay of after mixing AT 20 MIN.. RESULTES Uniformity

Sample no: 1 2 3 Average std. Dev. Range RSD LCL UCL

Temperature

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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 Capacity :_________________________ :_________________________ : ______________________lt. : _______________kg/lot. : 20 minutes : slow : As outlined in the batch manufacturing record. : Samples to be drawn at of 20 minutes, 30 minutes, & 40 minutes of mixing from Date:___________________

Ingredients and sequence of material addition: ____________________
Total weight of ingredients Mixing time Setting – stirrer Procedure Plan 3 different locations

FOR OIL PHASE SOLUTION TANK-RESULTS. Assay of after mixing AT 20 MIN.. RESULTES Uniformity

BATCH NO:

Sample no: 1 2 3 Average std. Dev. Range RSD LCL UCL

Temperature

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 Uniformity

Sample no: 1 2 3 Average std. Dev. Range RSD LCL UCL

Temperature

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 Mixing time Setting – stirrer Procedure Plan 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 BATCH NO: REMARK : _______________kg/lot. : 20 minutes : slow : As outlined in the batch manufacturing record. : Samples to be drawn at of 20 minutes, 30 minutes, & 40 minutes of mixing

Assay of after mixing AT 30 MIN.. Sample no: PH 1 2 3 Average std. Dev. Range RSD LCL UCL

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 Procedure Plan : slow ( R.P.M._________) : As outlined in the batch manufacturing record. : 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: Initional ( 0 time) Every 2 hours Immediately after the break time At the end of filling Average std. Dev. Range RSD LCL UCL APPEARANCE BATCH NO: WEIGHT IDENTIFICATION ASSAY TEST

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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

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 Average std. Dev. Range RSD LCL UCL POINTS Method of analysis adopted Ref No.: Analyst: Date Meet acceptance criteria. YES ( ) NO ( ) APPEARANCE WEIGHT IDENTIFICATION TEST ASSAY

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 2

S.S 350 Octagonal Steam Jacketed Tank. S.S 350 Octagonal Steam Jacketed Tank. ( OIL PHASE)

3 4 6

500 Octagonal Steam Jacketed Tank Storage Vessel Filling ,crimping & Coding machine

UTILITIES: 1 2 3 4 5 6 AHU SYSTEM WATER SYSTEM COMPRESSED AIR STEAM LIGHTNING 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.

2

3

Sample A (known amount of analysis. 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.

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SR Parameters

Type of sample 25 % of A 50 % of A 75 % of A 100 % of A 125 % of A Sample A1 15 min. degradation

Actual reading

Observed reading

Analysis Analysis performed checked by by

Ref. Work sheet

4

Linearity and range Response concentration curve on graph paper. 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

5

Sample A2 30 min. degradation

6

Sample A3 45 min. degradation 0.1 % of A 1% of A 5 % of A 10 % of A 20 % of A Method A Method B Method C

7

Analysis method (for non pharmacopoeial to be performed by other public lab.

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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.

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