Standard Operating Procedure for Validation of In-Process Testing for Capsules
| Department | Capsule Manufacturing |
|---|---|
| SOP No. | SOP/CM/180/2025 |
| Supersedes | SOP/CM/180/2022 |
| Page No. | Page 1 of 9 |
| Issue Date | 01/02/2025 |
| Effective Date | 05/02/2025 |
| Review Date | 01/02/2026 |
1. Purpose
The purpose of this SOP is to establish the procedure for validating in-process testing during capsule manufacturing. In-process testing ensures that the manufacturing process consistently meets product quality standards. This SOP ensures that in-process tests are reliable, accurate, and suitable for monitoring critical quality attributes throughout the production process.
2. Scope
This SOP applies to the validation of in-process tests used in the production of capsules, including tests for weight uniformity, hardness, dissolution, content uniformity, and other critical quality attributes. It covers all aspects of in-process testing from sample collection to result documentation and corrective actions for out-of-specification results.
3. Responsibilities
- Quality Control (QC) Team: Responsible for performing in-process tests, ensuring proper sample collection, conducting necessary tests, and documenting results accurately.
- Quality Assurance (QA) Team: Responsible for reviewing and approving the in-process testing procedures, protocols, and results to ensure compliance with GMP and regulatory standards.
- Production Team: Ensures that in-process testing is conducted at specified stages of production and that corrective actions are taken when deviations occur.
- Engineering Team: Responsible for ensuring that the equipment used in in-process testing is calibrated and maintained in accordance with regulatory standards.
4. Accountability
The QA Manager is accountable for overseeing the validation of in-process testing and ensuring that it meets regulatory and quality standards. The QC Supervisor is responsible for the execution and documentation of in-process tests. The Production Supervisor ensures that in-process testing is carried out at the designated stages of production.
5. Procedure
5.1 Pre-Validation Setup
Before initiating the validation process for in-process testing, ensure the following steps are completed:
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Review Validation Plan
- Review and approve the in-process testing validation plan, including the test parameters, methods, and acceptance criteria. Ensure that the validation plan is approved by the QA department before implementation.
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Define In-Process Test Parameters
- Identify the critical quality attributes that will be tested in-process, such as capsule weight, hardness, dissolution, and content uniformity. Ensure these tests are representative of the final product quality.
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Prepare In-Process Samples
- Prepare representative samples of capsules from various stages of the production process, ensuring they accurately represent the full range of variability (e.g., low, high, and normal values for weight and content uniformity).
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Calibrate Testing Equipment
- Ensure that all equipment used for in-process testing, such as hardness testers, dissolution apparatus, and balances, are calibrated according to the manufacturer’s specifications. Document calibration details in the Equipment Calibration Log (Annexure 1).
5.2 In-Process Testing Validation
Perform the following steps to validate the in-process testing methods:
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Test Execution
- Perform the in-process tests on the prepared samples. The tests should include parameters such as weight variation, content uniformity, hardness, dissolution, and visual inspection for defects.
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Critical Parameter Monitoring
- Ensure that each in-process test is conducted at the appropriate stage of production (e.g., after capsule filling, before sealing, after drying). Monitor parameters such as capsule weight, size, and hardness to detect any deviations from specified limits.
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Test Data Analysis
- Analyze the results of the in-process tests to confirm that they meet the defined acceptance criteria. If any test results are out-of-specification (OOS), immediately initiate corrective actions and investigate the cause.
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Documentation of Results
- Document all in-process test results in the In-Process Test Log (Annexure 2). This should include test parameters, results, and any deviations or corrective actions taken.
5.3 Post-Validation Activities
After the in-process testing validation is complete, ensure the following actions are taken:
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Approval of Results
- The QA Manager reviews the in-process testing results and ensures that they meet all specifications. Approve the validation results for use in routine production.
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Personnel Training
- Train the production and QC teams on the validated in-process testing procedures, including how to perform the tests, interpret results, and handle deviations.
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Routine Monitoring
- Implement routine monitoring of in-process tests during production. Ensure that all tests are carried out as per the validated procedures and that deviations are investigated and resolved.
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Documentation and Record Keeping
- Archive all in-process testing documentation, including the test logs, calibration records, and deviation reports, in compliance with regulatory retention requirements.
6. Abbreviations
- SOP: Standard Operating Procedure
- GMP: Good Manufacturing Practice
- QA: Quality Assurance
- QC: Quality Control
- R&D: Research and Development
- RH: Relative Humidity
- OOS: Out of Specification
7. Documents
- Annexure 1: Equipment Calibration Log
- Annexure 2: In-Process Test Log
- Annexure 3: In-Process Test Results Report
8. References
- FDA Guidance on In-Process Testing and Controls
- Good Manufacturing Practice (GMP) Guidelines
- USP <1225> – Validation of Compendial Methods
9. SOP Version
Version: 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | |||
| Designation | |||
| Department |
11. Annexures
Annexure 1: Equipment Calibration Log
| Equipment ID | Calibration Date | Operator | Calibration Details | Next Calibration Due |
|---|---|---|---|---|
| Capsule Hardness Tester 320 | 01/02/2025 | John Doe | Calibration of force and test speed | 01/02/2026 |
Annexure 2: In-Process Test Log
| Sample ID | Test Date | Test Type | Results | Remarks |
|---|---|---|---|---|
| Sample 001 | 02/02/2025 | Weight Uniformity | Pass | Within acceptable limits |
Annexure 3: In-Process Test Results Report
| Batch ID | Test Date | Test Parameters | Results | Deviation |
|---|---|---|---|---|
| Batch 001 | 02/02/2025 | Content Uniformity | Pass | None |
12. Revision History
| Revision Date | Revision No. | Revision Details | Reason for Revision | Approved By |
|---|---|---|---|---|
| 01/01/2024 | 1.0 | Initial version of SOP | Creation of SOP for in-process testing validation | QA Head |
| 01/02/2025 | 2.0 | Added new testing methods and updated parameters | Enhancement of test procedures and standardization | QA Head |