process. The report ensures traceability, scientific justification, and regulatory compliance as per ICH Q2(R1) and GMP expectations.

2. Scope

This SOP is applicable to all analytical methods developed for APIs, intermediates, excipients, and finished products within the Analytical Method Development (AMD) department and intended for validation, transfer, or regulatory filing.

3. Responsibilities

• Analytical Scientist: Drafts the Method Development Report using raw data and approved protocol.
• Team Leader: Reviews the draft report for accuracy, completeness, and data integrity.
• QA: Verifies compliance with documentation practices and SOP alignment.
• Head – AMD: Authorizes the final MDR for archival and subsequent validation activity.

4. Accountability

The Head of AMD is accountable for ensuring that every method developed is accompanied by a well-documented and approved Method Development Report before it is submitted for validation or transfer.

5. Procedure

5.1 Prerequisites

1. Ensure that method development activities were initiated with an approved Method Development Protocol (MDP).
2. Collect all experimental records, chromatograms, trial sheets, and optimization data.
3. Retrieve protocol and assign report number: MDR/YY/XXX (where YY = year, XXX = serial number).

5.2 Report Structure

1. Prepare the report as per the standard template in Annexure-1. The report should include:
   • Title and Document Number
   • Objective
   • Scope
   • Reference to MDP
   • Product and Analyte Information
   • Summary of Trials and Observations
   • Forced Degradation Studies (if applicable)
   • Optimization and Final Method Parameters
   • System Suitability Criteria
   • Conclusion
   • Annexures: Chromatograms, Data Tables, Graphs

5.3 Data Compilation

1. Summarize all major method trials and include:
   • Mobile phase trials
   • Buffer pH and ionic strength changes
   • Column screening and retention behavior
   • Detection optimization
2. Provide scientific rationale for the selected method condition.
3. Tabulate results in Annexure-2: Trial Summary Table.

5.4 Evaluation of Stability Indicating Capability

1. If applicable, summarize results from forced degradation studies:
   • Stress conditions and degradation observed
   • Peak purity results
   • Resolution from degradants
2. Include overlaid chromatograms in annexures.

5.5 Documentation of Final Method

1. Clearly document the final optimized method in Annexure-3: Final Method Parameters.
2. Include:
   • Column details
   • Mobile phase composition
   • Flow rate
   • Injection volume
   • Detection wavelength
   • System suitability criteria

5.6 Review and Approval

1. Submit draft MDR to Team Lead and QA for review.
2. Revise based on feedback and finalize.
3. Sign-off required by Analytical Scientist, Team Lead, QA, and Head – AMD.
4. Attach approval sheet as Annexure-4.

5.7 Archival

1. Submit final signed MDR to QA for archival in document control system.
2. Link MDR with MDP and upcoming validation protocol.
3. Log entry in Annexure-5: MDR Tracking Register.

6. Abbreviations

• MDR: Method Development Report
• MDP: Method Development Protocol
• QA: Quality Assurance
• HPLC: High Performance Liquid Chromatography
• PDA: Photodiode Array
• Rs: Resolution

7. Documents

1. Method Development Report Template – Annexure-1
2. Trial Summary Table – Annexure-2
3. Final Method Parameters – Annexure-3
4. Approval Sheet – Annexure-4
5. MDR Tracking Register – Annexure-5

8. References

• ICH Q2(R1) – Validation of Analytical Procedures
• ICH Q8 – Pharmaceutical Development
• WHO TRS 996 – Good Documentation Practices

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 Development Report Template

Section	Content
Objective	To develop and finalize an assay method for Metformin API
Scope	Applicable to development batch and subsequent commercial scale

Annexure-2: Trial Summary Table

Trial No.	Condition Modified	Result	Decision
1	Mobile Phase: Phosphate Buffer:ACN 60:40	Tailing = 2.4	Rejected
3	pH Adjusted to 3.5	Rs = 2.3	Accepted

Annexure-3: Final Method Parameters

Parameter	Condition
Column	C18, 250×4.6mm, 5µm
Mobile Phase	0.1% OPA:ACN 55:45
Flow Rate	1.0 mL/min
Detection	UV 232 nm
Injection Volume	10 µL

Annexure-4: Approval Sheet

Role	Name	Signature	Date
Prepared By
Checked By
Approved By

Annexure-5: MDR Tracking Register

MDR No.	Product	Initiation Date	Status	Archived
MDR/25/009	Paracetamol Tablets	14/05/2025	Approved	Yes

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Expanded trial tables and added MDR tracker	Documentation upgrade