scientific soundness.

2. Scope

This procedure applies to all AMD personnel responsible for selecting and justifying analytical techniques for the qualitative and quantitative evaluation of drug substances, drug products, intermediates, raw materials, and excipients.

3. Responsibilities

• AMD Scientist: Evaluates analyte characteristics and proposes analytical technique options.
• Team Lead: Reviews technique suitability, feasibility, and alignment with project requirements.
• QA: Verifies that the technique selection is justified and documented appropriately.
• Head – AMD: Approves the final selected technique based on risk, cost, and performance factors.

4. Accountability

The Head of Analytical Method Development is accountable for ensuring that the selection of analytical techniques is scientifically justified, well-documented, and consistent with regulatory and project needs.

5. Procedure

5.1 Define the Analytical Objective

1. Clarify the purpose of the analysis:
   • Identification
   • Assay (quantitative)
   • Impurity profiling
   • Dissolution testing
   • Stability indicating analysis
2. Refer to Quality Target Product Profile (QTPP) and Analytical Target Profile (ATP) when applicable.

5.2 Understand the Physicochemical Properties of the Analyte

1. Review the following attributes:
   • Molecular weight
   • Solubility
   • pKa and logP
   • UV absorbance or fluorescence characteristics
   • Thermal stability
2. Document key attributes in Annexure-1: Analyte Profile Sheet.

5.3 Evaluate Available Analytical Techniques

1. List applicable techniques for the specific objective:
   • Chromatographic: HPLC, UPLC, GC, TLC
   • Spectroscopic: UV-Vis, IR, NMR, Fluorescence
   • Titrimetric: Acid-base, redox, non-aqueous
   • Thermal Analysis: DSC, TGA
   • Elemental Analysis: AAS, ICP-MS
2. Consider detection limits, linearity, accuracy, and precision of each method.
3. Prepare a technique comparison matrix using Annexure-2.

5.4 Consider Practical Feasibility

1. Evaluate:
   • Availability of equipment
   • Calibration and validation status
   • Analyst proficiency and training level
   • Sample preparation complexity
   • Cost of analysis and throughput
2. Perform risk assessment if necessary using institutional risk templates.

5.5 Final Selection and Documentation

1. Document the rationale for technique selection, including a summary of rejected techniques and reasons.
2. Obtain approval from QA and Head – AMD.
3. Include this rationale in the Method Development Protocol and later in the Method Validation Report.

5.6 Re-Evaluation and Updates

1. If the method fails to meet performance criteria during development or validation, reassess the technique selection.
2. Document changes and approvals in Annexure-3: Re-evaluation Log.

6. Abbreviations

• AMD: Analytical Method Development
• ATP: Analytical Target Profile
• QTPP: Quality Target Product Profile
• HPLC: High Performance Liquid Chromatography
• GC: Gas Chromatography
• UV-Vis: Ultraviolet-Visible Spectroscopy
• SOP: Standard Operating Procedure

7. Documents

1. Analyte Profile Sheet – Annexure-1
2. Technique Comparison Matrix – Annexure-2
3. Re-evaluation Log – Annexure-3

8. References

• ICH Q2(R1) – Validation of Analytical Procedures
• ICH Q8 – Pharmaceutical Development
• WHO Technical Report Series 970

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Analyte Profile Sheet

Analyte Name	Molecular Weight	Solubility	pKa	Detection Wavelength
Losartan Potassium	461.01	Soluble in methanol	4.9	206 nm

Annexure-2: Technique Comparison Matrix

Technique	Specificity	LOD (µg/mL)	Time per Sample	Cost per Sample	Remarks
HPLC	High	0.1	12 mins	Rs. 100	Preferred method
UV-Vis	Moderate	1.0	5 mins	Rs. 30	Limited for impurities

Annexure-3: Re-evaluation Log

Date	Reason for Re-evaluation	Updated Technique	Approved By
05/04/2025	Low resolution in HPLC	UPLC	QA Head

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Expanded annexures and added re-evaluation tracking	Internal QA Audit