methods for raw materials, in-process samples, and finished injectable products.

3. Responsibilities

• Analytical Development Scientist: Designs and executes method development protocols.
• QC Analyst: Supports method transfer and evaluation.
• QA: Reviews method validation reports and ensures compliance.

4. Accountability

The Head – Analytical Development and Head – QA are accountable for the approval and control of developed methods.

5. Procedure

5.1 Pre-development Assessment

• Review available literature, regulatory references (USP, Ph. Eur., ICH), and innovator methods.
• Conduct pre-formulation studies to identify potential analytical challenges (e.g., degradation, interference).

5.2 Method Development Design

1. Define method objectives: assay, content uniformity, impurities, dissolution, pH, osmolality, etc.
2. Select suitable analytical technique: HPLC, GC, UV-Vis, potentiometry, TOC, etc.
3. Choose appropriate detection mode: UV, PDA, MS, fluorescence, RI, etc.
4. Identify key critical method parameters (CMPs): column type, mobile phase, flow rate, temperature, etc.

5.3 Optimization and Evaluation

1. Develop multiple trial methods using DoE (Design of Experiments) where feasible.
2. Evaluate parameters: specificity, linearity, accuracy, precision, robustness.
3. Use placebo and stress-degraded samples to confirm specificity and stability indicating nature.

5.4 Method Validation

Perform formal method validation as per ICH Q2(R1) covering:

• Specificity
• Linearity and range
• Accuracy
• Precision (repeatability and intermediate)
• Detection and quantitation limit
• Robustness and system suitability

Document results in Method Validation Report (Annexure-1).

5.5 Documentation

• Prepare Method Development Summary Report (Annexure-2).
• Prepare Standard Test Procedure (STP) and Analytical Method Validation Protocol.
• Archive raw data, chromatograms, spectra, and calculations.

5.6 Method Transfer (if applicable)

• Coordinate with the QC lab to transfer validated method.
• Conduct method transfer qualification/verification in the receiving lab.

6. Abbreviations

• HPLC: High Performance Liquid Chromatography
• DoE: Design of Experiments
• ICH: International Council for Harmonisation
• CMPs: Critical Method Parameters

7. Documents

1. Method Validation Report – Annexure-1
2. Method Development Summary Report – Annexure-2
3. STP Document – Annexure-3

8. References

• ICH Q2(R1) – Validation of Analytical Procedures
• USP General Chapter <1225> – Validation of Compendial Procedures
• Ph. Eur., IP Monographs

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation	Analytical Scientist	QA Executive	Head QA
Department	Analytical Development	Quality Assurance	Quality Assurance

11. Annexures

Annexure-1: Method Validation Report

Comprehensive data and observations from formal method validation activity.

Annexure-2: Method Development Summary Report

Summarizes trial runs, optimization rationale, and method selection decision tree.

Annexure-3: Standard Test Procedure (STP)

Final approved method for routine use with version number and effective date.

Revision History

Revision Date	Revision No.	Details	Reason	Approved By
15/01/2022	1.0	Initial SOP	New injectable line launch	Head QA
18/06/2025	2.0	Updated per ICH Q14 concepts	Regulatory alignment	Head QA