Standard Operating Procedure for Validation of Stability Studies for Capsules
| Department | Capsule Manufacturing |
|---|---|
| SOP No. | SOP/CM/177/2025 |
| Supersedes | SOP/CM/177/2022 |
| 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 stability studies for capsules. Stability testing is essential to determine the shelf-life of capsules, ensuring their safety, efficacy, and quality over time. This SOP outlines the requirements for designing, conducting, and analyzing stability studies to meet regulatory requirements and GMP standards.
2. Scope
This SOP applies to the stability studies conducted on capsules to assess their physical, chemical, microbiological, and performance attributes during storage. It covers all aspects of stability testing, including test conditions, time points, and parameters for capsules that are intended for long-term, accelerated, or real-time stability testing.
3. Responsibilities
- Quality Control (QC) Team: Responsible for conducting stability tests on the capsules as per the protocol, analyzing the results, and maintaining accurate records of the testing process.
- Quality Assurance (QA) Team: Reviews and approves the stability study protocols, results, and reports to ensure compliance with GMP and regulatory requirements. They also ensure that the results are appropriately documented and maintained.
- Regulatory Affairs: Ensures that the stability study protocols and results comply with the relevant regulatory guidelines and that stability data is available for product registration.
- R&D Team: Supports in designing the stability study protocols and assists in determining the appropriate conditions for the study based on product characteristics.
4. Accountability
The QA Manager is accountable for ensuring that the stability study protocols are followed and that the results meet the required specifications. The QC Supervisor is responsible for the execution of the stability testing and ensuring that the studies are completed on time with proper documentation.
5. Procedure
5.1 Pre-Study Setup
Before starting the stability studies, ensure the following steps are completed:
-
Review Stability Study Protocol
- Review and approve the stability study protocol, including the required test parameters, time points, and acceptance criteria. The protocol should be approved by the QA department prior to execution.
-
Select Stability Conditions
- Define the storage conditions based on the product’s requirements, such as temperature, humidity, and light exposure. Typical conditions include 25°C/60% RH for long-term stability and 40°C/75% RH for accelerated studies.
-
Prepare Stability Samples
- Prepare representative samples of the capsules to be tested, ensuring that the samples reflect the typical batch characteristics, including the correct batch number and manufacturing date.
-
Calibrate Testing Equipment
- Ensure that all testing equipment, such as stability chambers, temperature and humidity controllers, and testing instruments (e.g., HPLC, dissolution testers), are calibrated according to the manufacturer’s specifications.
5.2 Stability Study Execution
Follow these steps to execute the stability study:
-
Sample Storage
- Store the stability samples under the defined conditions (e.g., temperature and humidity) in the stability chambers. Ensure that the samples are placed in proper storage containers that prevent contamination.
-
Periodic Sampling
- At predefined time points (e.g., 0, 3, 6, 9, 12 months), remove a portion of the samples from storage for testing. Ensure that the samples are handled in a manner that maintains their integrity.
-
Test Parameters
- Test the samples for the required stability parameters, including:
- Physical appearance (e.g., color, texture, shape)
- Chemical stability (e.g., assay of active ingredient, degradation products)
- Microbial contamination (e.g., total aerobic microbial count, mold, and yeast)
- Dissolution performance
- Test the samples for the required stability parameters, including:
-
Analyze Test Results
- Analyze the results of the stability tests and compare them with the acceptance criteria. If any results fall outside the acceptable limits, investigate the cause and take corrective actions if necessary.
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Document Study Results
- Document the results of each stability test in the Stability Study Report (Annexure 1). This includes a detailed analysis of each parameter tested and any deviations from expected results.
5.3 Post-Study Activities
Once the stability study is completed, ensure the following actions are taken:
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Review and Approval of Results
- The stability study report should be reviewed and approved by the QA Manager to ensure compliance with GMP and regulatory requirements. Ensure that the report includes all relevant data, analysis, and conclusions.
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Prepare Final Stability Report
- Prepare the final stability report, including recommendations for the product’s shelf-life, storage conditions, and retest intervals based on the study findings. Submit the report to regulatory authorities if required.
-
Archive Study Documentation
- Archive all stability study documentation, including the study protocol, test results, and reports, in accordance with regulatory retention requirements. Ensure that the documentation is readily accessible for audits and inspections.
6. Abbreviations
- SOP: Standard Operating Procedure
- GMP: Good Manufacturing Practice
- QA: Quality Assurance
- QC: Quality Control
- RH: Relative Humidity
- HPLC: High-Performance Liquid Chromatography
- USP: United States Pharmacopeia
7. Documents
- Annexure 1: Stability Study Report
- Annexure 2: Stability Study Protocol
- Annexure 3: Test Results Log
8. References
- FDA Guidance on Stability Testing of Drug Products
- 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: Stability Study Report
| Batch ID | Test Date | Test Type | Results | Remarks |
|---|---|---|---|---|
| Batch 001 | 02/02/2025 | Potency Test | Pass | Stability meets the criteria for 12-month shelf-life |
Annexure 2: Stability Study Protocol
| Protocol ID | Study Start Date | Test Parameters | Acceptance Criteria |
|---|---|---|---|
| Protocol 001 | 01/01/2025 | Potency, dissolution, microbial load | Pass at 12-month, 25°C/60% RH |
Annexure 3: Test Results Log
| Sample ID | Test Date | Test Type | Results | Deviation |
|---|---|---|---|---|
| Sample 001 | 02/02/2025 | Dissolution Test | 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 stability studies in capsule manufacturing | QA Head |
| 01/02/2025 | 2.0 | Added new study conditions and test parameters | Improvement of stability study criteria | QA Head |