Standard Operating Procedure for Shelf-Life Testing Protocol of Elixir Formulations
| Department | Elixir Department |
|---|---|
| SOP No. | SOP/ELX/236/2025 |
| Supersedes | SOP/ELX/236/2022 |
| Page No. | Page 1 of 8 |
| Issue Date | 11/04/2025 |
| Effective Date | 15/04/2025 |
| Review Date | 11/04/2026 |
1. Purpose
To establish a standardized procedure for the design, execution, and evaluation of shelf-life testing of elixir formulations under prescribed storage conditions in order to determine product stability and expiry dating.
2. Scope
This SOP applies to the Quality Control and Stability Study teams involved in the assessment of shelf-life for elixir dosage forms during product development, registration, and post-marketing surveillance.
3. Responsibilities
- Stability Coordinator:
- Develop and execute the shelf-life testing protocol as per ICH guidelines.
- Ensure timely sample pulls and coordination with the QC lab.
- QC Analyst:
- Perform all assigned stability tests and record results as per validated methods.
- QA Officer:
- Ensure regulatory compliance, review final reports, and approve shelf-life assignment.
4. Accountability
The QC Head is accountable for timely and accurate testing. The QA Head is responsible for regulatory adherence and approval of expiry date assignment.
5. Procedure
5.1 Stability Study Design
- Design shelf-life testing protocol in accordance with ICH Q1A(R2) guidelines.
- Include both accelerated and long-term storage conditions:
- 25°C ± 2°C / 60% RH ± 5% RH (Long-term)
- 40°C ± 2°C / 75% RH ± 5% RH (Accelerated)
- Use three primary batches for marketed products or one pilot batch for development phase.
5.2 Time Points
- Long-term: 0, 3, 6, 9, 12, 18, 24, and 36 months (as applicable)
- Accelerated: 0, 3, and 6 months
- Intermediate (if required): 0, 6, and 12 months
5.3 Parameters Tested
- Appearance, color, clarity
- Assay of active ingredient
- Degradation products
- pH
- Viscosity
- Microbial limit tests
- Preservative and alcohol content (if applicable)
5.4 Data Analysis
- Graph assay and degradation over time and evaluate trend.
- Determine shelf-life as the point where API falls below 90% of labeled claim or when degradants exceed limit.
- Use Arrhenius equation if extrapolation from accelerated data is needed.
5.5 Reporting and Shelf-Life Assignment
- Prepare shelf-life report summarizing all data, trends, and graphical plots.
- QA reviews and signs off on shelf-life recommendation.
- Submit report for regulatory filing or internal shelf-life assignment.
5.6 Storage and Monitoring
- Store samples in validated stability chambers with continuous monitoring.
- Record daily temperature and humidity using data loggers.
- Initiate deviation if temperature excursions occur.
6. Abbreviations
- SOP: Standard Operating Procedure
- API: Active Pharmaceutical Ingredient
- QC: Quality Control
- QA: Quality Assurance
- ICH: International Council for Harmonisation
7. Documents
- Shelf-Life Study Protocol (Annexure-1)
- Stability Data Sheet
- Final Shelf-Life Report
8. References
- ICH Q1A(R2) – Stability Testing of New Drug Substances and Products
- WHO Technical Report Series No. 1010, Annex 10
- 21 CFR Part 211.166 – Stability Testing
9. SOP Version
Version: 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | |||
| Designation | |||
| Department |
11. Annexures
Annexure-1: Shelf-Life Study Protocol
| Study Title | Batch No. | Storage Condition | Time Points | Parameters | Prepared By |
|---|---|---|---|---|---|
| Elixir Shelf-Life Assessment | ELX-0425-052 | 25°C/60% RH | 0, 3, 6, 9, 12, 18, 24 months | Assay, Degradants, pH, Viscosity, Color | Rajesh Kumar |
Revision History:
| Revision Date | Revision No. | Revision Details | Reason for Revision | Approved By |
|---|---|---|---|---|
| 01/01/2024 | 1.0 | Initial SOP Release | New SOP Creation | QA Head |
| 11/04/2025 | 2.0 | Included intermediate storage and ICH alignment | Regulatory Compliance | QA Head |