TABLE OF CONTENTS
- Pre-approval Protocol
- Objective
- Scope
- Responsibility
- Validation Team training details
- Verification of Instruments for Calibration
- Reference of standard operating procedure/ Documents
- Validated Analytical Methods of intermediates for estimation of active ingredient
- Raw Material storage condition
- Hold time study Procedure
- Sampling size, plan, frequency, and Result/ observation
- Acceptance Criteria
- Details of deviation/ Non- compliance/ OOS
- Risk management study
- Summary of the study activity
- Recommendation
- Attachments
- Abbreviations
- Review and Post-approval
1. PRE-APPROVAL PROTOCOL
This document has been developed and the individuals listed below have reviewed the document and agree with its content and with their signature grant approval for its execution.
Functional Area | Name | Designation | Signature | Date |
PREPARED BY |
Validation QA | | | | |
REVIEWED BY |
Production Head | | | | |
QC Head | | | | |
Warehouse Head | | | | |
Engineering Head | | | | |
Quality Assurance | | | | |
APPROVED BY |
QA Head | | | | |
Plant Head | | | | |
2. OBJECTIVE
The objective of the hold time study is to establish the storage time of raw material with documented evidence.
3. SCOPE
This protocol is applicable for a hold-time study of raw materials used in manufacturing activity at PharmaGuide Ltd.
4. RESPONSIBILITY
4.1 Quality Assurance
- Preparation, Execution & reviewing the protocol.
- Collection of the samples as specified in the protocol.
- Reviewing the QC result and drawing a conclusion.
4.2 Quality Control
- Reviewing of hold time study protocol.
- Analyzing the hold time study samples as per this protocol and reporting the result.
4.3 Production
- Reviewing of hold time study protocol.
- To intimate the collection of samples of hold time study after completion of dispensing.
4.4 Warehouse
- Reviewing of hold time study protocol.
- To dispense the raw material required for hold time study.
4.5 Engineering
- Reviewing of hold time study protocol.
- Maintaining the required environmental condition of the storage area.
5. VALIDATION TEAM TRAINING DETAILS
The availability of training status and training records of all personnel involved in the validation/assessment exercise should be recorded.
DEPARTMENT | NAME | TRAINING STATUS | SIGNATURE |
Quality Assurance | | | |
Quality Control | | | |
Production | | | |
Warehouse | | | |
Engineering | | | |
6. VERIFICATION OF INSTRUMENTS FOR CALIBRATION
Sr. No. | Instrument Name | Instrument Code | Calibration Done on | Calibration Due on | Checked by Sign/Date |
1 | Weighing Balance | | | | |
7. REFERENCE OF STANDARD OPERATING PROCEDURE/DOCUMENTS
Sr. No. | SOP/Document Name | SOP/Doc. No. |
1. | SOP for Hold time study of products at different stages | - |
2. | SOP for Microbiological analysis of raw material, finished product, and Stability samples | - |
3. | SOP for Incident Reporting and Investigation | - |
4. | SOP for Deviation | - |
5. | SOP for Quality Risk Management | - |
6. | SOP for Handling of out of specification (OOS) results | - |
8. REFERENCE ANALYTICAL METHOD VALIDATION PROTOCOL NUMBER / QC SPECIFICATION No. TO BE RECORDED
Test | Analytical Method Validation Protocol No./QC specification number | Checked by (Sign/Date) |
Microbiological Analysis | | |
9. RAW MATERIAL STORAGE CONDITIONS
- Store the sample dispensed raw material in the fresh poly bag at a temperature of NMT 25℃ and Relative humidity of NMT 60%.
- Store the sample of dispensed raw material (moisture sensitive) in the fresh poly bag at a temperature of NMT 25℃ and Relative humidity of NMT 40%.
- Store the light-sensitive materials in a black poly bag.
10. HOLD TIME STUDY PROCEDURE
Selection of Raw Material:
The raw material shall be selected based on its nature and scientific rationale.
Dispensed Raw Material Details:
The raw materials used in the manufacturing of the batches selected for the Hold Time Study shall be tested, analyzed, and approved before use in the production as per their respective approved specifications. Details of the raw material shall be recorded in the report as shown below in the table.
Sampling Size, Plan, and Frequency:
Hold time study samples of raw materials shall be collected as per the below-mentioned quantity:
Sampling Plan for Dispensed Raw Material Hold Time Study |
Sr. No. | Storage Time | Test Parameters | Quantity of Sample | Acceptance Criteria |
1. | Initial (0) | Appearance Microbial test | 20 gm for every storage time Total Quantity: 60 gm | QC Test |
2. | 5th Day | Appearance Microbial test |
3. | 10th Day | Appearance Microbial test |
11. RESULT / OBSERVATION
12. ACCEPTANCE CRITERIA
Acceptance criteria for each raw material shall be as per the respective Quality Control specification for individual raw material.
13. DETAILS OF DEVIATION / NON-COMPLIANCE / OOS
_______________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________
14. RISK MANAGEMENT STUDY (If Any)
_______________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________
15. SUMMARY OF THE STUDY ACTIVITY
_______________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________
16. RECOMMENDATION
_______________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________
17. ATTACHMENTS
Attachment No. | Title of Attachment |
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18. ABBREVIATIONS
SOP: Standard operating procedure
OOS: Out of specification
QC: Quality Control
QA: Quality Assurance
No.: Number
Qty.: Quantity
S.No. : Serial number
G: Gram
19. REVIEW AND POST-APPROVAL
Functional area | Name | Designation | Signature | Date |
PERFORMED BY |
Validation QA | | | | |
Quality Control | | | | |
Production | | | | |
Warehouse | | | | |
Engineering | | | | |
Quality Assurance | | | | |
APPROVED BY |
QA Head | | | | |
Plant Head | | | | |
