Q2(R1) and GMP guidelines.

2. Scope

This SOP applies to all analytical scientists in the Analytical Method Development (AMD) department responsible for determining the viability of proposed or existing analytical methods for active pharmaceutical ingredients (APIs), formulations, raw materials, and intermediates.

3. Responsibilities

• Analytical Scientist: Conducts initial feasibility experiments and documents findings.
• Team Leader: Reviews feasibility results and determines whether method progression is justified.
• QA Department: Ensures documentation and compliance with internal and regulatory standards.
• Head – AMD: Approves final feasibility assessment report.

4. Accountability

The Head of Analytical Method Development is accountable for verifying that only feasible, robust, and regulatory-compliant methods proceed to formal development and validation stages.

5. Procedure

5.1 Initiation of Feasibility Study

1. Trigger feasibility assessment based on:
   • New product development
   • Regulatory filing needs
   • Technology transfer requirement
   • Alternative method proposal
2. Assign study to trained analyst with documented experience in the relevant technique.

5.2 Review of Available Information

1. Gather available method details from:
   • Pharmacopoeias (USP, IP, BP)
   • Published literature and patents
   • Vendor or prior client data
   • Internal method archives
2. Document review results in Annexure-1: Source Evaluation Log.

5.3 Preliminary Laboratory Evaluation

1. Conduct exploratory runs to assess:
   • Peak shape and resolution
   • Solubility and sample prep feasibility
   • Retention time and interference
   • Baseline noise and system suitability
2. Use HPLC, GC, UV, or any applicable technique based on analyte nature.
3. Record test runs in Annexure-2: Feasibility Data Log.

5.4 Feasibility Assessment Parameters

1. Evaluate the method for:
   • Specificity – No interference from blank, matrix, or excipients
   • Linearity – R² ≥ 0.990 over expected concentration range
   • Precision – RSD ≤ 2% (for assay)
   • Recovery – 98–102% (as applicable)
2. Perform at least three replicates for assay evaluation to check repeatability.
3. Document raw chromatograms and reports in the study file.

5.5 Risk Identification

1. Identify potential limitations:
   • Co-eluting peaks
   • Insoluble analytes
   • Unstable reference standards
   • Instrumental compatibility
2. Log risks and mitigations in Annexure-3: Risk Observation Sheet.

5.6 Feasibility Decision and Reporting

1. Prepare summary of findings and preliminary method attributes.
2. Use Annexure-4: Feasibility Report Format to present the conclusion.
3. Submit report for QA review and Head – AMD approval.
4. If deemed unfeasible, document justification and recommend alternate approaches.

6. Abbreviations

• API: Active Pharmaceutical Ingredient
• RSD: Relative Standard Deviation
• HPLC: High-Performance Liquid Chromatography
• UV: Ultraviolet
• QA: Quality Assurance
• AMD: Analytical Method Development

7. Documents

1. Source Evaluation Log – Annexure-1
2. Feasibility Data Log – Annexure-2
3. Risk Observation Sheet – Annexure-3
4. Feasibility Report Format – Annexure-4

8. References

• ICH Q2(R1) – Validation of Analytical Procedures
• ICH Q9 – Quality Risk Management
• Pharmacopoeial Methods (USP, IP, BP)

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Source Evaluation Log

Source	Reference Title	Year	Reviewed By
USP 43	Assay for API X	2022	Rajesh Kumar
PubMed	Stability-indicating HPLC for API X	2021	Sunita Reddy

Annexure-2: Feasibility Data Log

Date	Run ID	Condition	Observation	Analyst
10/04/2025	FZL-001	60:40 ACN:Water, 1 mL/min	Baseline noise observed	Ajay Mehra

Annexure-3: Risk Observation Sheet

Risk Description	Impact	Mitigation	Status
Peak merging with placebo	High	Change mobile phase pH	Pending

Annexure-4: Feasibility Report Format

Parameter	Observation	Conclusion
Specificity	No interference observed	Pass
Precision	RSD = 1.6%	Acceptable
Linearity	R² = 0.994	Acceptable

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Expanded assessment criteria and added annexure tracking	Internal QA Review