SOP Guide for Pharma

Tablets: SOP for API Retention Time Validation for Tablets – V 2.0

Auditor

Tablets: SOP for API Retention Time Validation for Tablets – V 2.0

Standard Operating Procedure for API Retention Time Validation for Tablets

Department Quality Control
SOP No. SOP/TAB/115/2025
Supersedes SOP/TAB/115/2022
Page No. Page 1 of 7
Issue Date 01/03/2026
Effective Date 06/03/2026
Review Date 01/03/2027

1. Purpose

To define the procedure for validating the retention time of the active pharmaceutical ingredient (API) in tablet formulations using High-Performance Liquid Chromatography (HPLC), ensuring consistency and accuracy in API identification and quantification.

2. Scope

This SOP applies to the validation of retention times for the API in tablet formulations using HPLC. The method ensures that the retention time of the API is consistent with established specifications and provides reliable data for quality control and regulatory compliance.

3. Responsibilities

4. Accountability

The QC Manager is accountable for ensuring the accurate performance of retention time validation. The QA Manager is responsible for reviewing and approving the results to ensure consistency and reliability in API testing.

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5. Procedure

5.1 Sample Preparation

  1. Weigh an appropriate amount of tablet sample (usually 10 tablets) to obtain a representative quantity for testing.
  2. Crush the tablets to a fine powder using a mortar and pestle or mechanical grinder to ensure uniformity.
  3. Dissolve the powder in an appropriate solvent (e.g., methanol or acetonitrile) based on the solubility of the API, and filter the solution using a 0.45 µm filter.
  4. If necessary, dilute the solution to bring the concentration within the optimal range for HPLC analysis.

5.2 HPLC System Setup

  1. Ensure that the HPLC system is properly calibrated and the appropriate column is installed for API separation.
  2. Set up the mobile phase, flow rate, and other conditions (e.g., temperature, detection wavelength) based on the method validation specifications.
  3. Prime the system to ensure consistent flow and eliminate air bubbles in the pump or lines.

5.3 Retention Time Validation

  1. Inject a known standard of the API into the HPLC system to establish a baseline retention time under the selected conditions.
  2. Inject the prepared tablet sample and record the retention time for the API peak in the chromatogram.
  3. Compare the retention time of the tablet sample with that of the standard. The retention time should match within an acceptable range (typically ±5% of the standard’s retention time).
  4. Perform the test in triplicate to ensure reproducibility of the results.
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5.4 Data Analysis and Calculation

  1. Calculate the average retention time for the API from the triplicate injections.
  2. Ensure that the average retention time falls within the specified range of the standard’s retention time. Any significant deviations must be investigated.
  3. Document all observations and results, including chromatograms, retention time data, and any deviations from the expected results.

5.5 Acceptance Criteria

  1. The retention time of the API should be consistent with the standard within the allowable limits (±5%).
  2. If the retention time falls outside the acceptable range, initiate an investigation to identify potential issues, such as incorrect mobile phase composition, column problems, or sample contamination.
  3. Corrective actions should be taken as necessary, and re-testing should be performed once the issue is resolved.

5.6 Documentation and Record-Keeping

  1. Record all validation results, including chromatograms, retention time calculations, and observations in the batch record (Annexure-2).
  2. Ensure that all records are signed, dated, and stored according to the company’s record retention policy for future audits and inspections.
  3. Maintain raw data, including instrument logs, standard preparation details, and deviation reports, for regulatory compliance and future reference.

5.7 Post-Test Actions

  1. Clean the HPLC system and associated equipment to remove any residual sample and prevent cross-contamination between tests.
  2. Dispose of used samples, solvents, and reagents according to the company’s waste disposal procedures.
  3. Ensure that the HPLC system is calibrated and maintained according to the manufacturer’s guidelines and company SOPs.
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6. Abbreviations

7. Documents

  1. Batch Record (Annexure-2)
  2. Deviation Report (Annexure-1)

8. References

9. SOP Version

Version: 2.0

10. Approval Section

Prepared By Checked By Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Deviation Report

Deviation Date Batch Number Deviation Description Corrective Action Responsible Person
15/12/2025 Batch 001 Retention time variation beyond acceptable limit Re-calibrated HPLC system and re-tested Jane Smith

Annexure-2: Batch Record

Batch Number Sample Weight (g) API Retention Time (min) Result
Batch 001 100 g 8.5 min Pass

Revision History:

Revision Date Revision No. Revision Details Reason for Revision Approved By
01/01/2024 1.0 Initial Version New SOP Creation QA Head
01/02/2025 2.0 Updated retention time limits Improved precision and accuracy QA Head
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