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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 1 0F 25

FORMULATION LINE

: :

PRODUCT NAME : 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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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 2 0F 25

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 5 ACTIVITY Preparation of validation protocol Approval of Validation protocol Production of validation Batches Testing of validation samples & Preparation of validation report Approval of validation report. RESPONSIBILITY REMARKS

3.0 PROCESS DESCIRPTION / FLOW SHEET

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 3 0F 25

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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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 4 0F 25

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

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
WEIGHT / TUBE CRIPING CODING

FILLING , CRIPING & CODING

FINAL PACKING

4.0 EQUIPMENT / FACTORY.

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 5 0F 25

A detailed list of equipment used for validation together with the cleaning status will be provided in the manufacturing documents. 4.1 LIST OF SOPS , 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

4.2 DETAILS OF EQUIPMENT TO BE USED. EQUIPMENT BALANCE DETAILS TYPE : MODEL: CAPACITY: MANUACTURER: TAG.NO.: M.O.C. TYPE : Approved by Prepared by Checked by

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 6 0F 25

WATER PHASE S.S.TANK

OIL PHASE TANK :

MFG. TANK :

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.

EQUIPMENT STORAGE TANK:

TUBE FILLING MACHINE:

TRANSFER PUMP:

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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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 7 0F 25

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
EXCIPIENT

WEIGHT/TUBE

PH

COOLING TEMPERATURE

TEMPERATURE

SPEED LOAD SIZE BOILING TEMPERATURE Prepared by WATER PHASE SOLUTION PREPARATION LOAD SIZE

SPEED

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MANUFACTURING

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 8 0F 25

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) 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)

Oil phase uniformity

Active ingredient uniformity

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

1. Weight of tube 2. Crimping

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 9 0F 25

CRITICAL PROCESS VARIABLE: SR 1 2 3 4 PROCESS / VARIABLE Water Phase Solution Preparation Oil Phase Solution Preparation Manufacturing Filling MACHINE SETTING (CONTROL VARIABLES) Quantity of water Setting and conditions as mentioned in Quantity of paraffin & wax the batch manufacturing record to be & other oil. Mixing time Cooling Time Speed, weight / tube. followed. REMARKS

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 10 0F 25

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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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 11 0F 25

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 After the completion of Oil phase solution , N=1 sample ( pooled from different locations) 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 assembly, consisting of transfer pump & holding tank and filling

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. Record the pH and assay of active content .

Oil phase solution preparation

MANUFACTURING PH, ASSAY

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 ( SIZE , LOCATION, TIME)

ACCEPTANCE CRITERIA

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 12 0F 25

Water phase solution preparation Oil phase solution preparation Manufacturing


ASSAY PH

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

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

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:

6.0 RECORDING OF DATA & DATA TREATMENT

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 13 0F 25

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:- 14 0F 25

DATA RECORDING SHEET #1 WATER 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 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:

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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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 15 0F 25

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 Prepared by Checked by

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 16 0F 25

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 Date:___________________

Ingredients and sequence of material addition: ____________________


Total weight of ingredients Mixing time Setting stirrer Procedure Plan from 3 different locations

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 Checked 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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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 18 0F 25

DATA RECORDING SHEET # 3 MANUFACTURING : 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 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

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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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 19 0F 25

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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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 20 0F 25

DATA RECORDING SHEET # 4 FILLING & CRIMPING : Equipment Name Identification no Capacity Setting stirrer Procedure Plan 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 :_________________________ :_________________________ : ______________________lt. : 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: Date:___________________

Mixing time( filling hopper) : Continues stirring during filling

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 21 0F 25

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____________________ Approved by Prepared by Checked by

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PROTOCOL NO: BATCH NO. QUALITY ASSURANCE DEPTT PAGE NO:- 22 0F 25

DATA RECORDING SHEET # 5 DATE:____________________


SR NAME OF CRITICAL EQUIPMENT/UTILITIES QUALIFICATION/ VALIDATION FILE REF.NO. DATE OF QUALIFICATION / VALIDATION

1 2 3 4 6

S.S 350 Octagonal Steam Jacketed Tank. S.S 350 Octagonal Steam Jacketed Tank. ( OIL PHASE) 500 Octagonal Steam Jacketed Tank Storage Vessel 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 1 Accuracy % Recovery of known amount. Type of sample Sample A (known amount of analysis. Approved by Prepared by Checked by Actual reading Observed reading Analysis performed by Analysis checked by Ref. Work sheet

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PROTOCOL NO: BATCH NO. 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 4 Linearity and range Response concentration curve on graph paper.

Type of sample 25 % of A 50 % of A 75 % of A 100 % of A 125 % of A

Actual reading

Observed reading

Analysis Analysis performed checked by by

Ref. Work sheet

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Specificity/ selectivity( by larger communication of analytical method.) for identification of impurities assay of active component etcTemp & 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

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

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 Checked by

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