Standard Operating Procedure for Precision and Repeatability Assessment in Method Validation
| Department | Analytical Method Development |
|---|---|
| SOP No. | SOP/AMD/200/2025 |
| Supersedes | SOP/AMD/200/2022 |
| Page No. | Page 1 of 14 |
| Issue Date | 19/05/2025 |
| Effective Date | 20/05/2025 |
| Review Date | 19/05/2026 |
1. Purpose
To define a systematic procedure for evaluating the precision and repeatability of an analytical method during method validation as per ICH Q2(R2) guidelines.
2. Scope
This SOP applies to all quantitative analytical methods developed and
validated within the Analytical Method Development (AMD) department, including assay, dissolution, impurity profiling, and content uniformity tests.
3. Responsibilities
- Analytical Scientist: Designs the precision study and interprets data.
- Validation Analyst: Executes replicate sample analysis across same-day and inter-day conditions.
- QA Officer: Verifies compliance and reviews final precision report.
- Head – AMD: Authorizes the precision evaluation and report for regulatory use.
4. Accountability
The Head of AMD is accountable for ensuring that the precision and repeatability assessments meet acceptable statistical and regulatory criteria.
5. Procedure
5.1 Repeatability Assessment
- Prepare six individual test solutions from the same homogeneous sample batch.
- Analyze each solution under identical conditions using the validated method.
- Record peak area, retention time, and concentration in Annexure-1: Repeatability Data Sheet.
- Calculate:
- Mean
- Standard Deviation (SD)
- Relative Standard Deviation (%RSD)
5.2 Intermediate Precision (Ruggedness)
- Repeat analysis using:
- Different analysts
- Different instruments
- Different days (minimum 2)
- Use same sample preparation protocol for each analyst.
- Record all observations in Annexure-2: Intermediate Precision Summary.
- Compare results across sets using statistical tools such as ANOVA.
5.3 Acceptance Criteria
- Repeatability: %RSD should be ≤ 2.0% for assay methods.
- Intermediate Precision: %RSD across all variables should be ≤ 3.0%.
- Results must be consistent and within specification limits.
5.4 Reporting
- Prepare a consolidated report summarizing:
- Repeatability results
- Intermediate precision results
- Acceptance status
- Attach chromatograms and instrument printouts.
- Summarize results in Annexure-3: Precision Validation Summary Report.
6. Abbreviations
- RSD: Relative Standard Deviation
- SD: Standard Deviation
- SOP: Standard Operating Procedure
- AMD: Analytical Method Development
- ANOVA: Analysis of Variance
- ICH: International Council for Harmonisation
7. Documents
- Repeatability Data Sheet – Annexure-1
- Intermediate Precision Summary – Annexure-2
- Precision Validation Summary Report – Annexure-3
8. References
- ICH Q2(R2) – Validation of Analytical Procedures
- FDA Guidance – Analytical Procedures and Methods Validation
- Internal AMD Quality Manual
9. SOP Version
Version: 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | |||
| Designation | |||
| Department |
11. Annexures
Annexure-1: Repeatability Data Sheet
| Sample No. | Peak Area | Calculated Result (%) |
|---|---|---|
| 1 | 543210 | 99.2% |
| 2 | 541890 | 98.9% |
| 3 | 545000 | 99.5% |
| 4 | 542100 | 99.0% |
| 5 | 543800 | 99.3% |
| 6 | 544200 | 99.4% |
Annexure-2: Intermediate Precision Summary
| Day | Analyst | Instrument | Average Result (%) |
|---|---|---|---|
| Day 1 | Rajesh Kumar | HPLC-01 | 99.1% |
| Day 2 | Sunita Reddy | HPLC-02 | 98.8% |
Annexure-3: Precision Validation Summary Report
| Parameter | Result | Acceptance Criteria | Status |
|---|---|---|---|
| Repeatability (%RSD) | 0.45% | ≤ 2.0% | Pass |
| Intermediate Precision (%RSD) | 0.72% | ≤ 3.0% | Pass |
Revision History:
| Revision Date | Revision No. | Details | Reason | Approved By |
|---|---|---|---|---|
| 04/05/2025 | 2.0 | Added intermediate precision criteria and annexures for statistical reporting | Regulatory alignment |