expectations (ICH Q14/Q10), and consistent performance throughout the method’s operational life.

2. Scope

This SOP applies to all analytical methods developed, validated, transferred, or used for release, stability, and in-process testing across the Analytical Method Development (AMD) department and any quality control (QC) units that adopt such methods.

3. Responsibilities

• Analytical Scientist: Initiates and documents method development, validation, and monitoring data.
• Team Lead: Ensures compliance across method lifecycle stages and monitors performance trend reports.
• QA: Reviews and approves lifecycle documents and tracks method changes and deviations.
• Head – AMD: Approves lifecycle decisions, including method retirement or revalidation.

4. Accountability

The Head of Analytical Method Development is accountable for establishing, maintaining, and reviewing method lifecycle systems to ensure analytical control and scientific justification across the method’s use.

5. Procedure

5.1 Phase 1: Method Development

1. Define Analytical Target Profile (ATP) and use QbD principles where applicable.
2. Perform risk assessment and conduct trials using DoE or traditional approaches.
3. Document in Method Development Protocol and Report (refer to SOP/AMD/013 and 014).
4. Maintain development data in Annexure-1: Method Lifecycle Master Register.

5.2 Phase 2: Method Validation

1. Prepare validation protocol per ICH Q2(R1) or Q14 (for enhanced approach).
2. Validate parameters including:
   • Specificity
   • Linearity
   • Accuracy and precision
   • LOD/LOQ
   • Robustness
3. Obtain QA approval and record summary in Annexure-2: Method Validation Summary.

5.3 Phase 3: Technology Transfer

1. Transfer the validated method to the receiving lab using a predefined protocol.
2. Perform comparative analysis and generate transfer report.
3. Log outcomes in Annexure-3: Method Transfer Record.

5.4 Phase 4: Routine Usage and Performance Monitoring

1. Apply the method for release and stability testing.
2. Track performance trends:
   • System Suitability (e.g., Rs, tailing, RT)
   • OOS/OOT investigations
   • Repeat testing frequency
3. Summarize monthly/quarterly reviews in Annexure-4: Method Performance Monitoring Log.

5.5 Phase 5: Change Control and Revalidation

1. Evaluate impact of any change to method, material, instrument, or SOP on method performance.
2. If significant, trigger partial or full revalidation.
3. Document decision in Annexure-5: Method Change Impact Assessment.

5.6 Phase 6: Method Retirement

1. Retire method when:
   • Superseded by a new method
   • Product is discontinued
   • Regulatory requirement changes
2. Submit retirement proposal to QA and HOD.
3. Archive all documentation and update Annexure-6: Method Retirement Record.

6. Abbreviations

• ATP: Analytical Target Profile
• QbD: Quality by Design
• OOT: Out of Trend
• OOS: Out of Specification
• DoE: Design of Experiments
• MODR: Method Operable Design Region

7. Documents

1. Method Lifecycle Master Register – Annexure-1
2. Method Validation Summary – Annexure-2
3. Method Transfer Record – Annexure-3
4. Method Performance Monitoring Log – Annexure-4
5. Method Change Impact Assessment – Annexure-5
6. Method Retirement Record – Annexure-6

8. References

• ICH Q10 – Pharmaceutical Quality System
• ICH Q14 – Analytical Procedure Development
• ICH Q2(R1) – Validation of Analytical Procedures
• USP General Chapter <1224> – Transfer of Analytical Procedures

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 Lifecycle Master Register

Method ID	Product	Status	Initiated By	Date
MTH/2025/031	Metformin Tablets	Validated	Ajay Mehra	10/04/2025

Annexure-2: Method Validation Summary

Parameter	Result	Criteria	Status
Accuracy	99.5%	98–102%	Pass

Annexure-3: Method Transfer Record

Receiving Lab	Date	Transfer Outcome	Remarks
QC Unit – Baddi	12/05/2025	Successful	Minor adjustment in injection volume

Annexure-4: Method Performance Monitoring Log

Date	Parameter	Observed Value	Trend	Remarks
15/05/2025	RT	7.82 min	Within Range	Stable

Annexure-5: Method Change Impact Assessment

Change Description	Impact Level	Revalidation Required	QA Decision
Column brand change	Medium	Yes (partial)	Approved

Annexure-6: Method Retirement Record

Method ID	Retirement Reason	Effective Date	Approved By
MTH/2019/002	Superseded by new UHPLC method	01/03/2025	QA Head

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Expanded lifecycle stages; added annexures for trend monitoring and retirement	ICH Q14 lifecycle alignment