GMP and ICH Q2(R1) guidelines.

2. Scope

This SOP applies to all validated and development-stage analytical methods evaluated for ruggedness and robustness within the Analytical Method Development lab for both API and formulation projects.

3. Responsibilities

• Analyst: Performs ruggedness and robustness studies and records observations.
• Section In-Charge: Reviews results and ensures adherence to protocol.
• QA Representative: Verifies data and approves reports for regulatory submission.
• Department Head: Approves protocols and ensures overall compliance.

4. Accountability

The Head of Analytical Method Development is accountable for implementation and periodic review of ruggedness and robustness evaluations.

5. Procedure

5.1 Ruggedness Evaluation

1. Prepare the analytical method validation protocol including ruggedness parameters such as:
   • Different analysts
   • Different instruments
   • Different days
   • Different laboratories (if applicable)
2. Analyze at least six replicates under each condition.
3. Calculate system precision (RSD%) and compare across variables.
4. Document findings in the Ruggedness Evaluation Report (Annexure-1).

5.2 Robustness Evaluation

1. Identify critical parameters that could affect method performance such as:
   • Flow rate (±10%)
   • Mobile phase pH (±0.2 units)
   • Column temperature (±5°C)
   • Injection volume (±10%)
2. Perform analysis with deliberate variations in each parameter.
3. Compare retention time, resolution, peak shape, and recovery with standard conditions.
4. Ensure RSD is within 2% and system suitability passes under each condition.
5. Document results in the Robustness Evaluation Log (Annexure-2).

5.3 Data Handling and Documentation

1. All chromatograms, system suitability reports, and data calculations shall be retained.
2. Prepare summary reports indicating observed variability and justification of acceptance criteria.
3. Obtain QA review before final approval.

5.4 Report Review and Approval

1. The compiled report must be reviewed by a senior analyst and approved by the Department Head.
2. Forward the final report to QA for archiving.

6. Abbreviations

• SOP: Standard Operating Procedure
• QA: Quality Assurance
• RSD: Relative Standard Deviation
• ICH: International Council for Harmonisation
• HPLC: High Performance Liquid Chromatography

7. Documents

1. Ruggedness Evaluation Report – Annexure-1
2. Robustness Evaluation Log – Annexure-2
3. System Suitability Checklist – Annexure-3

8. References

• ICH Q2(R1): Validation of Analytical Procedures
• WHO TRS 996: Quality Assurance of Pharmaceuticals
• GMP Guidelines for Analytical Method Validation

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name	Rajesh Kumar	Meena Pillai	Sunita Reddy
Designation	Sr. Analyst	QA Reviewer	AMD Head
Department	AMD	QA	Analytical Method Development

11. Annexures

Annexure-1: Ruggedness Evaluation Report

Analyst	Date	Instrument	RSD%	Remarks
Anjali Singh	01/05/2025	HPLC-101	1.3	Accepted
Ramesh Pawar	02/05/2025	HPLC-103	1.5	Accepted

Annexure-2: Robustness Evaluation Log

Parameter	Condition	Result	RSD%	Conclusion
Flow Rate	0.9 mL/min	RT 5.2 min	1.2	Pass
Flow Rate	1.1 mL/min	RT 4.8 min	1.4	Pass

Annexure-3: System Suitability Checklist

Test ID	Retention Time	Resolution	Theoretical Plates	Status
SST-001	5.0	2.5	4500	Pass
SST-002	4.9	2.4	4300	Pass

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
21/05/2025	2.0	Complete SOP rewrite per ICH Q2(R1)	Annual Review	Sunita Reddy
15/03/2022	1.0	Initial Release	New SOP	Department Head