Standard Operating Procedure for Verification of Analytical Procedures in AMD
| Department | Analytical Method Development |
|---|---|
| SOP No. | SOP/AMD/313/2025 |
| Supersedes | SOP/AMD/313/2022 |
| Page No. | Page 1 of 11 |
| Issue Date | 01/06/2025 |
| Effective Date | 03/06/2025 |
| Review Date | 01/06/2026 |
1. Purpose
This SOP defines the step-by-step process for verifying analytical procedures prior to their adoption in routine quality control testing. The objective is to confirm that the method is suitable for its intended use under actual laboratory conditions.
2. Scope
This SOP applies to
the verification of compendial methods (e.g., USP, EP, IP) and established non-compendial methods used in the Analytical Method Development (AMD) laboratory, particularly when adopted from literature or transferred from another site.
3. Responsibilities
- Analyst: Executes the verification experiments and records all data.
- AMD Reviewer: Evaluates results and ensures compliance with the verification protocol.
- QA Unit: Reviews the final verification report and authorizes method implementation.
4. Accountability
The Head of Analytical Method Development is accountable for ensuring that no analytical procedure is implemented without documented verification in accordance with this SOP.
5. Procedure
5.1 Verification Planning
- Determine whether verification is required based on risk assessment (see Annexure-1).
- Prepare a Verification Protocol outlining the scope, parameters to be verified, acceptance criteria, and rationale.
- Get protocol approved by AMD and QA prior to execution.
5.2 Parameters to be Verified
- Accuracy: Recovery studies using known concentrations of API or reference standard.
- Precision: Repeatability and intermediate precision using RSD calculation.
- Specificity: Demonstrated absence of interference from excipients or impurities.
- LOD/LOQ: As applicable based on method type (typically for non-compendial methods).
- Linearity: Correlation coefficient (r² ≥ 0.99) across concentration range.
5.3 Execution of Verification
- Follow the approved protocol strictly for sample and standard preparation.
- Ensure equipment calibration and environmental conditions are suitable.
- Document all chromatograms, calculations, observations, and deviations.
- Record data in the Verification Worksheet (Annexure-2).
5.4 Evaluation of Results
- Compare observed results against acceptance criteria defined in the protocol.
- Perform statistical analysis where necessary to support conclusions.
- Summarize outcomes in Verification Report Template (Annexure-3).
5.5 Handling of Deviations
- Any deviation during execution must be recorded in the Deviation Log (Annexure-4).
- Conduct a root cause analysis and assess its impact on verification outcome.
- Implement CAPA as necessary and document the resolution.
5.6 Approval and Implementation
- Submit Verification Report for review by QA and AMD head.
- Upon approval, update the Analytical Method Registry and assign Method ID.
- Release the method for routine use by QC or AMD teams.
6. Abbreviations
- API: Active Pharmaceutical Ingredient
- QA: Quality Assurance
- RSD: Relative Standard Deviation
- LOD: Limit of Detection
- LOQ: Limit of Quantitation
7. Documents
- Verification Protocol Template – Annexure-1
- Verification Worksheet – Annexure-2
- Verification Report Format – Annexure-3
- Deviation Log Format – Annexure-4
8. References
- ICH Q2(R1): Validation of Analytical Procedures
- USP <1226>: Verification of Compendial Procedures
- FDA Guidance for Industry: Analytical Procedures and Methods Validation
9. SOP Version
Version: 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | Anju Sharma | Priya Nair | Dr. Harshita Goyal |
| Designation | AMD Analyst | QA Reviewer | Head – Analytical Method Development |
| Department | Analytical Method Development | Quality Assurance | Analytical Method Development |
11. Annexures
Annexure-1: Verification Protocol Template
Details rationale, method overview, parameters selected for verification, and acceptance criteria with justification.
Annexure-2: Verification Worksheet
Tabulated results for accuracy, precision, specificity, and linearity with test run dates, analyst initials, and instrument IDs.
Annexure-3: Verification Report Format
Includes executive summary, method description, test results, conclusions, and recommendations for implementation.
Annexure-4: Deviation Log Format
| Deviation ID | Description | Impact | CAPA | Status |
|---|---|---|---|---|
| DEV-313-01 | Outlier in accuracy recovery for Level 2 | Minor | Re-analysis and SOP training | Closed |
Revision History:
| Revision Date | Revision No. | Details | Reason | Approved By |
|---|---|---|---|---|
| 01/06/2025 | 2.0 | Inclusion of risk assessment and updated worksheet formats | Annual SOP Review | Dr. Harshita Goyal |
| 15/08/2022 | 1.0 | Initial Issue | New SOP | QA Head |