Procedure for Long-Term Stability Testing
| Department | Quality Control (QC)/Quality Assurance (QA)/Research & Development (R&D) |
|---|---|
| SOP No. | SOP/Ointment/102 |
| Supersedes | V 1.0 |
| Page No. | Page X of Y |
| Issue Date | [Insert Issue Date] |
| Effective Date | [Insert Effective Date] |
| Review Date | [Insert Review Date] |
1. Purpose
The purpose of this Standard Operating Procedure (SOP) is to define the procedure for conducting long-term stability testing of ointments to assess their physical, chemical, and microbiological stability over an extended period under recommended storage conditions.
2. Scope
This SOP applies to all personnel in the Quality Control (QC), Quality Assurance (QA), and Research & Development (R&D) departments responsible for executing, monitoring, and documenting long-term stability studies.
3. Responsibilities
- QC Analyst: Conducts stability testing at predefined intervals.
- QC Supervisor: Ensures compliance with the stability study protocol.
- QA Officer: Reviews stability study data and ensures adherence to guidelines.
- R&D Scientist: Analyzes data trends and recommends formulation adjustments if needed.
- QA Manager: Approves stability study protocols and ensures regulatory compliance.
4. Accountability
The QA and QC Managers are accountable for ensuring that long-term stability testing is conducted as per ICH Q1A(R2) guidelines.
5. Procedure
5.1 Preparation for Stability Testing
- Ensure the stability study protocol is approved before initiating the study.
- Select representative ointment batches for testing.
- Label samples with batch number, manufacturing date, and storage conditions.
- Store samples under recommended long-term conditions as per
ICH guidelines (e.g., 25°C ± 2°C/60% RH ± 5% RH or 30°C ± 2°C/65% RH ± 5% RH, depending on regulatory requirements).
5.2 Stability Testing Parameters
- Physical Properties: Assess changes in appearance, color, odor, and texture.
- Chemical Stability: Analyze the active ingredient content using validated analytical methods.
- Microbiological Testing: Perform microbial limit tests for contamination.
- pH Measurement: Evaluate changes in pH levels over time.
- Viscosity Analysis: Determine changes in consistency and spreadability.
5.3 Sampling Intervals
- Collect samples for testing at predefined intervals: 0, 3, 6, 9, 12, 18, 24, and 36 months.
- Perform all tests as per the approved stability study protocol.
- Record observations and test results in the Stability Testing Log.
5.4 Handling Out-of-Specification (OOS) Results
- Identify deviations from acceptance criteria.
- Initiate an Out-of-Specification (OOS) investigation if required.
- Implement corrective and preventive actions (CAPA) as necessary.
5.5 Documentation and Data Analysis
- Record test results in the Stability Study Report.
- Ensure data integrity and traceability.
- QA must review and approve stability data before finalizing the report.
6. Abbreviations
- GMP – Good Manufacturing Practices
- QA – Quality Assurance
- QC – Quality Control
- ICH – International Council for Harmonisation
- RH – Relative Humidity
- OOS – Out-of-Specification
7. Documents
- Stability Testing Log (Annexure-1)
- Long-Term Stability Study Report (Annexure-2)
8. References
- ICH Q1A(R2) Stability Testing of New Drug Substances and Products
- WHO GMP Guidelines for Pharmaceutical Stability Studies
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 Testing Log
| Date | Batch Number | Storage Condition | Testing Interval | Parameter Tested | Result | Reviewed By |
|---|---|---|---|---|---|---|
| 01/02/2025 | OINT-201 | 25°C/60% RH | 6 Months | Viscosity | Compliant | QA Officer |
| 01/08/2025 | OINT-201 | 25°C/60% RH | 12 Months | pH | Stable | QA Officer |
Annexure-2: Long-Term Stability Study Report
| Batch Number | Study Start Date | Study End Date | Test Parameters | Results | Final Conclusion |
|---|---|---|---|---|---|
| OINT-201 | 01/02/2025 | 01/02/2028 | pH, Viscosity, Microbial Limits | Compliant | Meets Stability Criteria |
| OINT-202 | 01/03/2025 | 01/03/2028 | Appearance, Assay, Microbial Limits | Compliant | Meets Stability Criteria |
12. Revision History:
| Revision Date | Revision No. | Details of Revision | Reason for Revision | Approved By |
|---|---|---|---|---|
| 01/01/2024 | 1.0 | Initial Version | New SOP | QA Head |
| 01/02/2025 | 2.0 | Updated SOP Format | Standardization of Document | QA Head |