and days on method performance, in accordance with ICH Q2(R1).

2. Scope

This SOP applies to all analytical methods under development and validation that require intermediate precision evaluation as part of method validation protocols, for both APIs and finished dosage forms.

3. Responsibilities

• Analysts: Perform experiments under specified conditions and record data accurately.
• Group Leader: Design the intermediate precision protocol and review experimental data.
• QA Reviewer: Review raw data, approve compliance to acceptance criteria, and verify results.
• Department Head: Ensure proper implementation and documentation of intermediate precision studies.

4. Accountability

The Department Head of Analytical Method Development is accountable for ensuring intermediate precision studies are conducted per approved protocols and regulatory standards.

5. Procedure

5.1 Protocol Design

1. Prepare an Intermediate Precision Study Protocol including:
   • Objective
   • Materials and equipment required
   • Experimental design
   • Acceptance criteria (e.g., RSD ≤ 2.0%)
2. Get the protocol reviewed and approved by QA before execution.

5.2 Experimental Setup

1. Perform analysis of six replicate preparations by:
   • At least two different analysts
   • Using at least two different instruments
   • On two or more different days
2. Ensure consistent sample batch and standard preparation.

5.3 Data Recording

1. Document:
   • Analyst name
   • Instrument ID
   • Date and time of analysis
   • All chromatograms and assay data
2. Calculate % Assay for each replicate and RSD for each set.
3. Record in Annexure-1: Intermediate Precision Data Log.

5.4 Evaluation and Acceptance

1. Evaluate results across all variables to ensure:
   • RSD ≤ 2.0%
   • No significant analyst or instrument bias
2. Investigate and document deviations, if any.
3. Summarize results in Annexure-2: Intermediate Precision Summary Report.

5.5 Documentation and Review

1. Compile all raw data and summary into a final report.
2. QA to verify and sign-off on the report.
3. Archive completed documents per data retention policy (minimum 5 years).

6. Abbreviations

• SOP: Standard Operating Procedure
• RSD: Relative Standard Deviation
• API: Active Pharmaceutical Ingredient
• QA: Quality Assurance
• ICH: International Council for Harmonisation

7. Documents

1. Intermediate Precision Data Log – Annexure-1
2. Intermediate Precision Summary Report – Annexure-2
3. Final QA Approved Study Report – Annexure-3

8. References

• ICH Q2(R1): Validation of Analytical Procedures
• WHO Technical Report Series 996
• US FDA Guidance on Analytical Procedure Validation

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name	Santosh Mehra	Divya Shah	Sunita Reddy
Designation	Sr. Analyst	QA Reviewer	Department Head
Department	Analytical Method Development	QA	Analytical Method Development

11. Annexures

Annexure-1: Intermediate Precision Data Log

Analyst	Instrument ID	Date	Replicate No.	Assay %
Analyst A	HPLC-01	15/05/2025	1	98.7%
Analyst A	HPLC-01	15/05/2025	2	98.5%
Analyst B	HPLC-02	16/05/2025	3	98.6%
Analyst B	HPLC-02	16/05/2025	4	98.4%
Analyst A	HPLC-03	17/05/2025	5	98.8%
Analyst B	HPLC-01	17/05/2025	6	98.5%

Annexure-2: Intermediate Precision Summary Report

Mean Assay (%)	Standard Deviation	% RSD	Acceptance Criteria	Conclusion
98.58%	0.14	0.14%	≤ 2.0%	Pass

Annexure-3: Final QA Approved Study Report

Method Title	Assay of Cetirizine HCl
Verification Date	17/05/2025
Analysts	Santosh Mehra, Priya Nair
Conclusion	Method demonstrates acceptable intermediate precision.

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
21/05/2025	2.0	Expanded to include day/instrument variability	Annual Review	Sunita Reddy
05/03/2022	1.0	Initial Issue	New SOP	QA Head