Q2(R1), GMP, and WHO TRS 996.

2. Scope

This SOP applies to all compendial methods adopted for testing of raw materials, in-process samples, and finished products in the Analytical Method Development department.

3. Responsibilities

• Analyst: Executes method verification protocol and performs data recording.
• Section Lead: Prepares and reviews method verification plan and results.
• QA Executive: Reviews the verification report and approves documentation.
• Department Head: Ensures compliance and signs off the final report.

4. Accountability

The Department Head of AMD is accountable for ensuring the verification of pharmacopoeial methods before their routine use in the lab.

5. Procedure

5.1 Review of Pharmacopoeial Method

1. Review the selected monograph method from official compendia (e.g., USP, BP, IP).
2. Identify method parameters such as:
   • System suitability criteria
   • Chromatographic conditions
   • Sample and standard preparation
   • Diluent composition

5.2 Planning of Method Verification

1. Draft a Method Verification Protocol containing:
   • Objective and scope
   • Verification parameters: system suitability, accuracy, precision, specificity, LOD/LOQ (if applicable)
   • Acceptance criteria (based on monograph or internal standards)
   • List of reagents, columns, instruments, and materials
2. Review and approval of protocol by QA before execution.

5.3 Execution of Verification

1. Prepare system suitability standards and conduct runs to meet USP/EP/IP acceptance limits.
2. Perform:
   • Precision: minimum 6 replicate injections
   • Accuracy: recovery at 3 levels (80%, 100%, 120%)
   • Specificity: blank, placebo, and spiked samples
3. Document chromatograms and raw data in Annexure-1 and Annexure-2.

5.4 Evaluation and Reporting

1. Compile results in Annexure-3: Method Verification Report.
2. Ensure %RSD, recovery, and specificity data meet criteria as per pharmacopoeial standards.
3. Report any deviations and provide justification for acceptance or re-verification.

5.5 Approval and Archiving

1. QA reviews the compiled verification report and signs off if compliant.
2. Final report stored in the AMD archive for a minimum of 5 years.

6. Abbreviations

• SOP: Standard Operating Procedure
• QA: Quality Assurance
• USP: United States Pharmacopeia
• IP: Indian Pharmacopoeia
• BP: British Pharmacopoeia
• LOD: Limit of Detection
• LOQ: Limit of Quantification

7. Documents

1. Chromatographic Results Log – Annexure-1
2. Precision and Accuracy Worksheet – Annexure-2
3. Method Verification Report – Annexure-3

8. References

• ICH Q2(R1): Validation of Analytical Procedures
• GMP Guidelines – Schedule M (India)
• WHO Technical Report Series 996

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name	Neha Bhatt	Ajit More	Sunita Reddy
Designation	Sr. Scientist	QA Reviewer	AMD Head
Department	Analytical Method Development	QA	Analytical Method Development

11. Annexures

Annexure-1: Chromatographic Results Log

Injection No.	Peak Area	Retention Time	System Suitability Pass
1	1023456	5.03	Yes
2	1023401	5.01	Yes

Annexure-2: Precision and Accuracy Worksheet

Level	Recovery %	% RSD	Acceptance Criteria	Status
80%	98.5%	1.2%	95-105%	Pass
100%	99.8%	0.9%	95-105%	Pass
120%	101.2%	1.1%	95-105%	Pass

Annexure-3: Method Verification Report

Method Title	Assay of Ibuprofen – USP
Analyst	Neha Bhatt
Verification Date	15/05/2025
Verification Parameters	Precision, Accuracy, Specificity
Final Conclusion	Method suitable and verified for use

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
21/05/2025	2.0	Clarified scope, added Annexure-3	Annual Review	Sunita Reddy
10/03/2022	1.0	Initial Issue	New SOP	QA Head