sample matrix and calculating the percentage recovered. Accuracy is a key performance parameter during analytical method validation, ensuring the method’s ability to measure the true value of an analyte across a defined range.

2. Scope

This procedure is applicable to all new and existing analytical methods developed or validated for quantitative estimation of active pharmaceutical ingredients (API), excipients, finished dosage forms, and raw materials in the Analytical Method Development (AMD) laboratory.

3. Responsibilities

• Analytical Chemist: Prepares and analyzes accuracy solutions, records data, and performs calculations.
• AMD Scientist: Reviews and verifies raw data and calculations, evaluates accuracy results.
• Quality Assurance (QA): Verifies final report and ensures protocol adherence before approval.

4. Accountability

The Head of Analytical Method Development is accountable for implementation, compliance, documentation, and archiving of accuracy validation reports in accordance with ICH, WHO, and national regulatory standards.

5. Procedure

5.1 Preparation of Accuracy Samples

1. Select three levels of concentration—typically 50%, 100%, and 150% of target assay concentration.
2. Prepare placebo or blank matrix equivalent to the sample matrix used in routine analysis.
3. Spike the placebo with known quantities of standard (API) to obtain final concentrations at each level in triplicate.

5.2 Sample Analysis

1. Analyze the accuracy samples using the validated method or the method under development.
2. Inject all replicates into the instrument under the same chromatographic/analytical conditions.
3. Document the retention time, area, and calculated concentration of each injection.

5.3 Calculation and Evaluation

1. Calculate the % recovery using the formula:
   % Recovery = (Measured amount / Added amount) × 100
2. Calculate mean recovery and % relative standard deviation (%RSD) for each level.
3. Acceptance Criteria: 98.0%–102.0% for assay methods (as per ICH), with %RSD ≤ 2.0% unless otherwise justified.

5.4 Documentation

1. Enter all raw data into the Accuracy Recovery Summary Sheet (Annexure-1).
2. Attach chromatograms, calibration curve (if applicable), and sample preparation details.
3. Compile the accuracy section of the method validation report as per the AMD format.

6. Abbreviations

• API: Active Pharmaceutical Ingredient
• RSD: Relative Standard Deviation
• QA: Quality Assurance
• AMD: Analytical Method Development

7. Documents

1. Annexure-1: Accuracy Recovery Summary Sheet
2. Annexure-2: Sample Spiking Records
3. Method Validation Protocol and Report

8. References

• ICH Q2(R1): Validation of Analytical Procedures
• USP General Chapter <1225>: Validation of Compendial Procedures
• WHO TRS No. 996, Annex 7: Guidelines on Validation
• 21 CFR Part 211 – cGMP Guidelines

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name	Arvind Patil	Megha Shah	Dr. R.K. Joshi
Designation	Analyst	QA Officer	Head – AMD
Department	Analytical Method Development	Quality Assurance	Analytical Method Development

11. Annexures

Annexure-1: Accuracy Recovery Summary Sheet

Level	Added (%)	Recovered (%)	Mean Recovery	% RSD
Low (50%)	50.00	49.85	99.7%	0.22%
Mid (100%)	100.00	100.2	100.2%	0.18%
High (150%)	150.00	149.5	99.7%	0.25%

Conclusion: Accuracy results within acceptable limits across all levels. Method is accurate.

Annexure-2: Sample Spiking Records

Documented preparation of placebo, spike level calculations, and analyst signatures.

Revision History

Revision Date	Revision No.	Description	Reason	Approved By
01/06/2025	2.0	Enhanced acceptance criteria and updated annexures	Annual Review	Dr. R.K. Joshi
10/07/2022	1.0	Initial SOP Issuance	New SOP	QA Head