Procedure for Stability Testing Under Accelerated Conditions
| Department | Quality Control (QC)/Quality Assurance (QA)/Analytical Development |
|---|---|
| SOP No. | SOP/Ointment/069 |
| 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 method for conducting stability testing under accelerated conditions to evaluate the shelf-life, physical, chemical, and microbiological stability of ointments.
2. Scope
This SOP applies to all personnel in the Quality Control (QC), Quality Assurance (QA), and Analytical Development departments responsible for conducting accelerated stability testing of ointments during formulation development, validation, and routine batch release.
3. Responsibilities
- Quality Control Analyst: Conducts stability testing and records results.
- Quality Assurance Personnel: Reviews and approves test results.
- Stability Study Coordinator: Manages stability chamber conditions and sample tracking.
- R&D and Analytical Development Team: Evaluates formulation modifications based on stability test results.
4. Accountability
The QC, Stability Study, and QA Managers are accountable for ensuring that stability testing is conducted accurately and documented as per ICH and GMP guidelines.
5. Procedure
5.1 Equipment and Materials
- Stability chambers with temperature and humidity control
- HPLC system for assay and degradation analysis
- pH meter
- Viscometer
- Microbial testing equipment
- Data recording sheets
5.2 Sample Preparation
- Select representative samples from different production batches.
- Store samples in appropriate stability study containers.
- Label each sample with batch number, storage conditions, and testing intervals.
5.3 Stability Storage Conditions
- Accelerated Conditions: 40°C ± 2°C / 75% RH ± 5% for 6 months
- Intermediate Conditions (if required): 30°C ± 2°C / 65% RH ± 5% for 12 months
- Long-Term Conditions: 25°C ± 2°C / 60% RH ± 5% for 24 months
5.4 Stability Testing Parameters
5.4.1 Physical Tests
- Appearance: No color or texture changes should occur.
- Phase Separation: Check for oil-water phase separation.
- Viscosity: Measure using a viscometer.
5.4.2 Chemical Tests
- Assay: Determine API concentration using HPLC.
- Degradation Products: Analyze degradation peaks.
- pH: Ensure no significant variation from the initial value.
5.4.3 Microbiological Tests
- Total Aerobic Microbial Count (TAMC): Should comply with specifications.
- Total Yeast and Mold Count (TYMC): Should comply with specifications.
- Pathogen Testing: Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa should be absent.
5.5 Stability Testing Schedule
- Samples should be tested at the following intervals:
- Initial (T0)
- 1 Month (T1)
- 3 Months (T3)
- 6 Months (T6)
- For long-term studies, additional testing may be conducted at 9, 12, 18, and 24 months.
5.6 Acceptance Criteria
- No significant change in physical, chemical, or microbiological properties.
- API content should remain within ±5% of initial assay value.
- Degradation products should remain within acceptance limits.
5.7 Documentation
- Record all stability test results in the Stability Test Log.
- Document environmental conditions of the stability chambers.
- QA personnel must review and approve results before batch release.
6. Abbreviations
- GMP – Good Manufacturing Practices
- QA – Quality Assurance
- QC – Quality Control
- RH – Relative Humidity
- ICH – International Council for Harmonisation
7. Documents
- Stability Test Log (Annexure-1)
- Ointment Stability Report (Annexure-2)
8. References
- ICH Q1A(R2) – Stability Testing of New Drug Substances and Products
- WHO Stability Testing 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 Test Log
| Date | Batch Number | Storage Condition | Time Point | Assay (%) | pH | Viscosity | Result | Verified By |
|---|---|---|---|---|---|---|---|---|
| 01/02/2025 | OINT-101 | 40°C/75% RH | 3M | 98.5% | 6.2 | 45,000 cP | Pass | QA Officer |
| 02/02/2025 | OINT-102 | 40°C/75% RH | 6M | 97.2% | 6.1 | 44,500 cP | Pass | QA Officer |
Annexure-2: Ointment Stability Report
| Date | Batch Number | Storage Condition | Acceptance Criteria | Result | Final Status | Approved By |
|---|---|---|---|---|---|---|
| 01/02/2025 | OINT-101 | 40°C/75% RH | No significant change | Pass | Approved | QA Head |
| 02/02/2025 | OINT-102 | 40°C/75% RH | No significant change | Pass | Approved | QA Head |