Scope

This SOP applies to the planning of validation of analytical methods developed for drug substances, drug products, excipients, and cleaning validations intended for use in Quality Control or regulatory submissions.

3. Responsibilities

• Analytical Scientist: Designs validation strategy and drafts validation protocol.
• QA Officer: Reviews and approves validation plan to ensure compliance with regulatory standards.
• Validation Analyst: Executes validation activities as per approved protocol.
• Head – AMD: Approves validation plan and authorizes execution.

4. Accountability

The Head of AMD is accountable for ensuring validation plans are scientifically justified, protocol-driven, and aligned with global regulatory expectations.

5. Procedure

5.1 Method Categorization

1. Determine the type of analytical method:
   • Identification
   • Assay (Quantitative)
   • Impurity Testing
   • Limit Tests
   • Dissolution
   • Cleaning Validation
2. Refer to ICH Q2(R2) to identify applicable validation parameters.

5.2 Validation Parameter Planning

1. Based on method category, select validation characteristics:
   • Specificity
   • Linearity and Range
   • Accuracy
   • Precision (Repeatability and Intermediate Precision)
   • LOD/LOQ
   • Robustness
   • System Suitability
2. Ensure plan includes number of analysts, days, instruments, and concentrations to be tested.

5.3 Validation Protocol Development

1. Prepare a protocol including:
   • Objective and scope
   • Method summary
   • Validation parameters with acceptance criteria
   • Statistical tools and evaluation plan
   • List of equipment, reagents, and reference standards
2. Use Annexure-1: Method Validation Planning Template to structure protocol sections.
3. Submit to QA and Department Head for review and approval.

5.4 Execution and Schedule Planning

1. Create a Gantt chart or schedule identifying timelines, personnel, and milestones.
2. Ensure availability of:
   • Calibrated equipment
   • Qualified reference and working standards
   • Trained analysts
3. Document readiness in Annexure-2: Validation Preparation Checklist.

6. Abbreviations

• SOP: Standard Operating Procedure
• ICH: International Council for Harmonisation
• LOD: Limit of Detection
• LOQ: Limit of Quantification
• AMD: Analytical Method Development

7. Documents

1. Method Validation Planning Template – Annexure-1
2. Validation Preparation Checklist – Annexure-2

8. References

• ICH Q2(R2) – Validation of Analytical Procedures
• FDA Guidance – Analytical Procedures and Methods Validation
• Internal Quality Manual – Analytical Validation Planning

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 Validation Planning Template

Section	Details
Method Type	Assay of API
Validation Parameters	Specificity, Linearity, Accuracy, Precision, Robustness
Acceptance Criteria	R² ≥ 0.998; Recovery 98–102%; RSD ≤ 2%
Statistical Tool	ANOVA, Regression

Annexure-2: Validation Preparation Checklist

Item	Status	Remarks
Validated Equipment	Available	HPLC #0023 Calibrated
Qualified Analysts	Yes	Trained on SOP/AMD/196/2025
Standards Availability	Yes	Reference standard batch RS-A005

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Revised to include validation planning checklist and template-based protocol structure	Alignment with updated ICH Q2(R2)