changes in potency, degradation products, and overall quality over time.

2. Scope

This SOP applies to all drug substances and drug products handled by the Analytical Method Development (AMD) department, including tablets, capsules, injectables, and topical dosage forms, during stability studies under ICH-guided storage conditions.

3. Responsibilities

• Analytical Scientist: Designs, develops, and validates the shelf-life method based on product characteristics.
• Stability Analyst: Performs real-time and accelerated testing, logs data, and monitors trends.
• QA Officer: Ensures compliance with stability protocols and method validation requirements.
• Head – AMD: Approves method development report and authorizes application for stability use.

4. Accountability

The Head of AMD is accountable for the scientific soundness, regulatory alignment, and implementation of shelf-life determining methods during product development and lifecycle management.

5. Procedure

5.1 Method Design Criteria

1. Ensure the method is capable of detecting:
   • Decrease in assay (API content)
   • Increase in degradation products
   • Changes in physical properties (color, pH, viscosity)
2. Select method type (HPLC, UV, potentiometry, etc.) based on drug characteristics.

5.2 Stability Study Integration

1. Design method for use at all stability time points under:
   • Long-term (25°C ± 2°C / 60% RH ± 5%)
   • Accelerated (40°C ± 2°C / 75% RH ± 5%)
   • Intermediate (30°C ± 2°C / 65% RH ± 5%)
2. Ensure consistency in method application across batches and packaging configurations.

5.3 Validation Requirements

1. Validate the method as per ICH Q2(R2) guidelines covering:
   • Specificity – Distinguish API from impurities and excipients
   • Linearity – Correlation coefficient ≥ 0.998 across 80–120% range
   • Accuracy – Recovery within 98–102%
   • Precision – RSD ≤ 2% (intra- and inter-day)
   • Robustness – Evaluate variation in mobile phase pH, flow rate, and detection wavelength
2. Record validation data in Annexure-1: Method Validation Summary.

5.4 Shelf-Life Estimation and Trend Analysis

1. Plot assay and impurity results over time using appropriate statistical tools (e.g., regression analysis).
2. Estimate the time point where the assay or impurity exceeds ICH limits.
3. Determine shelf-life using linear or non-linear regression as applicable.
4. Summarize results in Annexure-2: Shelf-Life Estimation Report.

5.5 Report and Documentation

1. Compile data into a final development report, including:
   • Analytical method and SOP reference
   • Validation results and system suitability
   • Trend charts and shelf-life projection
2. Submit for QA review and archival.

6. Abbreviations

• API: Active Pharmaceutical Ingredient
• HPLC: High-Performance Liquid Chromatography
• SOP: Standard Operating Procedure
• ICH: International Council for Harmonisation
• RSD: Relative Standard Deviation

7. Documents

1. Method Validation Summary – Annexure-1
2. Shelf-Life Estimation Report – Annexure-2

8. References

• ICH Q1A(R2) – Stability Testing of New Drug Substances and Products
• ICH Q2(R2) – Validation of Analytical Procedures
• FDA Guidance for Industry – 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: Method Validation Summary

Parameter	Observed	Criteria	Status
Specificity	Resolved peaks	No interference	Pass
Linearity	R² = 0.9993	≥ 0.998	Pass
Accuracy	99.2%	98–102%	Pass
Precision	1.4%	≤ 2%	Pass

Annexure-2: Shelf-Life Estimation Report

Condition	Tested Timepoints	Assay Trend	Impurity Trend	Estimated Shelf-Life
25°C/60% RH	0M, 3M, 6M, 9M, 12M	-0.65%/month	+0.20%/month	24 Months

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Incorporated regression-based estimation and impurity profiling trend section	Alignment with updated ICH Q2(R2)