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HOLD TIME STUDY PROTOCOL FOR CETIZIN TABLET

BATCH SIZE: 1,000,000 TABLETS

THE ACME LABORATORIES LTD.

DHAMRAI, DHAKA
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PROTOCOLAPPROVAL
The following representatives, by signing and dating in the space provided below, have approved this
protocol for execution:
PREPARED BY:

Name Designation Signature Date

Miton Chowdhury Executive, Validation

REVIEWED BY:

Name Designation Signature Date

Mohammad Farhad Hossain Manager, QC

Jiban Chandra Das AGM, R&D

Md. Zahidul Islam Sr. AGM, Production

Sanzida Chowdhury Manager, Validation

APPROVED BY:
Name Designation Signature Date
Mahmudul Hasan Deputy Manager, QA

AUTHORIZED BY:

Name Designation Signature Date

Shah Sharfin Sr. Manager, QA

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Table of Contents
1. REVISION HISTORY........................................................................................................................................ 4
2. OBJECTIVE...................................................................................................................................................... 4
3. SCOPE.............................................................................................................................................................. 4
4. ASSOCIATED DOCUMENT.............................................................................................................................. 4
5. ABREVIATION.................................................................................................................................................. 5
6. RESPONSIBILITIES......................................................................................................................................... 5
6.1 Production Department............................................................................................................................. 5

6.2 Quality Control (QC)/ Microbiology Department........................................................................................ 5

6.3 Product development Department............................................................................................................ 5

6.4 Quality Assurance (QA) Department........................................................................................................ 6

6.5 Quality Operation...................................................................................................................................... 6

7. DESCRIPTION OF MANUFACTURING PROCEDURE....................................................................................6

8. SPECIFICATIONS FOR INTERMEDIATE AND BULK PRODUCTS IN DETAILS............................................9
9. SAMPLING AND TESTING STRATEGIES..................................................................................................... 12
9.1 Sampling Quantity & Testing Frequency................................................................................................. 12

9.2 Sampling Procedure............................................................................................................................... 12

9.3 Testing Requirement............................................................................................................................... 12

9.4 Testing Procedure.................................................................................................................................. 12

10. VALIDATION STRATEGIES........................................................................................................................... 13

11. STORAGE CONDITION.................................................................................................................................. 13
12. ACCEPTANCE CRITERIA.............................................................................................................................. 14
13. REVALIDATION REQUIREMENT................................................................................................................... 14
14. DEVIATION FORMS....................................................................................................................................... 14
15. APPENDICES................................................................................................................................................. 14
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APPENDIX –C
ANALYTICAL REPORT SHEET OF DISPENSED MATERIAL (CETIRIZINE
HYDROCHLORIDE BP)
Product Name : CETIZIN TABLET

Batch No. :

Date of Tested :

Test Parameters Acceptance Criteria Results

Description White or almost white powder.

A. Conform by IR.
Identification
B. A curdled, white precipitate will be formed
which is dissolved in ammonia soluiton.
Clear and not more intensely colored than
Appearance of solution
reference solution BY7
pH
Related substances
A. For each impurity not more than
A. Impurity A,B,C,D,E & F
0.15%
B. Unspecified impurity B. Not more than 0.10%
C. Total impurities C. Not more than 0.30%
Loss on drying Not more than 0.5%
Assay (As Cetirizine
Hydrochloride on dried 99.0% to 101.0%
basis)
Microbial Test
Total Aerobic Microbial Count
Not more than 103 cfu/g
(TAMC)
Total Combined Yeasts and
Not more than 102 cfu/g
Moulds Count (TYMC)
Escherichia coli Absent / 1g
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APPENDIX - E
ANALYTICAL REPORT SHEET OF DRY GRANULES

Product Name : CETIZIN TABLET

Batch No. :

Date of Tested :

Test Parameters Acceptance Criteria Result

Description White to off white color powder.

LOD at 105°C (1.80-3.00)% at 105⁰C

Microbial Test

Total Aerobic Microbial Count Not more than 103 cfu/gm

Total Yeast & Mold Count Not more than 102 cfu/gm

Escherichia Coli Absent

Checked By:_____________________________ Reviewed By:_____________________________

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APPENDIX -F
ANALYTICAL REPORT SHEET OF LUBRICATED GRANULES

Product Name : CETIZIN TABLET

Batch No. :

Date of Tested :

Test Parameters Acceptance Criteria Result

Description White to off white color granular powder.
Identification Complies by HPLC or UV
Cetirizine HCl Spectrophotometer
LOD at 105°C 1.80% - 3.00%
Assay (Cetirizine HCl BP) 90.0 % to 110.0%

Microbial Test

Total Aerobic Microbial Count Not more than 103 cfu/gm

Total Yeast & Mold Count Not more than 102cfu/gm

Escherichia coli Absent

Checked By:_________________________ Reviewed By:________________________

APPENDIX - G
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ANALYTICAL REPORT SHEET OF CORE TABLET

Product Name : CETIZIN TABLET

Batch No. :

Date Tested :

Test Parameters Specification Result

Description White round bi-convex tablets engraved

‘ACME’ on one face and a break line on
the other face.
Identification Complies by HPLC or UV
Cetirizine HCl Spectrophotometer

LOD at 1050C 1.80% - 3.00%

Assay (Cetirizine HCl BP) 90.0 % to 110.0% (9.0 mg -11.0mg)

Microbial Test

Total Aerobic Microbial Count Not more than 103 cfu/gm

Total Yeast & Mold Count Not more than 102cfu/gm

Escherichia coli Absent

Checked By:_________________________ Reviewed By:________________________

APPENDIX - G
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ANALYTICAL REPORT SHEET OF COATED TABLET

Product Name : CETIZIN TABLET

Batch No. :

Date Tested :

Test Parameters Specification Result

Description White round bi-convex film coated tablets

engraved ‘ACME’ on one face and a
break line on the other face.
Identification Complies by HPLC or UV
Cetirizine HCl Spectrophotometer

LOD at 1050C 1.80% - 3.00%

Dissolution Not less than 80.0%

Assay (Cetirizine HCl BP) 90.0 % to 110.0% (9.0 mg -11.0mg)

Microbial Test

Total Aerobic Microbial Count Not more than 103 cfu/gm

Total Yeast & Mold Count Not more than 102cfu/gm

Escherichia coli Absent

APPENDIX - H
DEVIATION FORM
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Report Identification Number

Description of deviation and date observed:

Initiated By: Signature: Date:

Corrective action to be taken:

Responsible Person For Action: Expected Date:

Corrective Action Proposed By: Date:

Corrective Action Approved By: Date:

Corrective Action taken:

Performed By: Date:

Verified By: Date:

APPENDIX - I
DEVIATION AND CORRECTIVE ACTION - SUMMARY
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Report Identification Nature of Deviation Sign-Off Date

Number

COMMENTS:

Compiled By: _________________________________________ Date:_______________________

Reviewed By:_________________________________________ Date: _______________________

APPENDIX - J
CERTIFICATE OF APPROVAL
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 Prepared By

Name Designation Signature

Summary:

Conclusion:

 Reviewed By

Name Designation Signature

 Approved By

Name Designation Signature

 Authorized By

Name Designation Signature