types.

2. Scope

This SOP applies to Analytical Method Development (AMD) scientists and associated personnel involved in designing and documenting analytical procedures for final product release and stability studies of pharmaceutical formulations.

3. Responsibilities

• AMD Scientist: Executes method development experiments for formulations and documents results.
• Team Leader: Reviews draft procedures and approves selected method parameters.
• QA Department: Reviews the method development documentation for completeness and compliance.
• Head – AMD: Authorizes the finalized method for validation or verification.

4. Accountability

The Head of AMD is accountable for ensuring that test procedures for formulations are developed using scientifically sound approaches and that they are suitable for regulatory submission and routine quality control.

5. Procedure

5.1 Preliminary Understanding of the Dosage Form

1. Review formulation details:
   • Dosage form (tablet, capsule, suspension, injection)
   • Strength and composition
   • Excipients used (diluents, binders, preservatives)
   • Intended use and packaging configuration
2. Summarize these attributes in Annexure-1: Formulation Profile Sheet.

5.2 Literature and Pharmacopoeial Review

1. Identify available pharmacopoeial monographs (USP, IP, BP, Ph.Eur) and relevant scientific publications.
2. Evaluate previous internal methods used for similar products or APIs.
3. Document key findings in Annexure-2: Reference Summary Table.

5.3 Development of Analytical Methods

1. Design method for the following critical quality attributes (CQAs):
   • Identification
   • Assay of active content
   • Related substances / degradation products
   • Uniformity of dosage units
   • Dissolution and disintegration (as applicable)
2. Select suitable techniques: HPLC, GC, UV, potentiometry, or titrimetry depending on the analyte.
3. Perform robustness testing by varying parameters such as pH, temperature, flow rate, and mobile phase composition.

5.4 Optimization and Standardization

1. Fine-tune method parameters based on:
   • System suitability (e.g., tailing factor, theoretical plates)
   • Precision and accuracy
   • Peak resolution and retention time
2. Record optimized conditions in Annexure-3: Method Development Log.

5.5 Preparation of Test Procedure Document

1. Draft the analytical procedure using Annexure-4: Draft Format for Test Procedure.
2. Include:
   • Objective
   • Scope
   • Principle
   • Equipment and reagents
   • Standard and sample preparation
   • System suitability
   • Calculation formulae
3. Ensure clarity and replicability by including necessary figures or chromatograms where applicable.

5.6 Internal Review and Approval

1. Submit the draft for internal review by Team Leader and QA.
2. Incorporate feedback and finalize the method.
3. Approval to be granted by the Head of AMD before initiating method validation.

5.7 Integration into Stability and QC Programs

1. Forward finalized method to Stability and Quality Control departments.
2. Ensure proper version control and training of end users prior to implementation.
3. Maintain archival copies and change control history as per QMS.

6. Abbreviations

• AMD: Analytical Method Development
• API: Active Pharmaceutical Ingredient
• HPLC: High Performance Liquid Chromatography
• USP/IP/BP: United States/Indian/British Pharmacopoeia
• QA: Quality Assurance
• CQA: Critical Quality Attribute
• QMS: Quality Management System

7. Documents

1. Formulation Profile Sheet – Annexure-1
2. Reference Summary Table – Annexure-2
3. Method Development Log – Annexure-3
4. Draft Format for Test Procedure – Annexure-4

8. References

• ICH Q2(R1) – Validation of Analytical Procedures
• ICH Q8 – Pharmaceutical Development
• WHO Technical Report Series 996
• Applicable Pharmacopoeial Monographs

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Formulation Profile Sheet

Product Name	Dosage Form	Strength	Excipients
Paracetamol Tablets	Tablet	500 mg	Lactose, Starch, PVP, Talc

Annexure-2: Reference Summary Table

Source	Title	Year	Reviewed By
USP 43	Paracetamol Monograph	2022	Sunita Reddy
Journal of Chromatography	RP-HPLC Method for Paracetamol	2021	Rajesh Kumar

Annexure-3: Method Development Log

Date	Parameter Optimized	Final Condition	Outcome
12/04/2025	Mobile Phase Composition	Phosphate buffer:ACN (60:40)	Improved peak shape

Annexure-4: Draft Format for Test Procedure

Section	Details
System Suitability	RSD < 2%, resolution > 2.0
Preparation	Standard: 500 mg in 100 mL, Sample: Powdered tablet equivalent to 500 mg
Calculation	% Assay = (Sample Area / Standard Area) × Std Weight / Sample Weight × 100

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Enhanced layout for multiple formulation types	Harmonization of formats