Tablets: SOP for HPLC Testing for Drug Content in Tablets – V 2.0

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Tablets: SOP for HPLC Testing for Drug Content in Tablets – V 2.0

Standard Operating Procedure for HPLC Testing for Drug Content in Tablets

Department Tablet
SOP No. SOP/TAB/092/2025
Supersedes SOP/TAB/092/2022
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 performing HPLC (High-Performance Liquid Chromatography) testing for drug content in tablets, ensuring that the active pharmaceutical ingredient (API) in tablets is within the specified limits and meets quality requirements.

2. Scope

This SOP applies to the determination of drug content in tablet formulations using HPLC, including preparation, calibration, and analysis of samples for compliance with specified API content.

3. Responsibilities

  • Manufacturing Personnel: Responsible for providing tablet samples for HPLC testing and ensuring proper handling and storage of the samples.
  • Quality Control (QC): Responsible for conducting the HPLC testing, preparing the samples, performing the analysis, and ensuring that the results comply with specifications.
  • Quality Assurance (QA): Ensures that the testing procedure is followed correctly and reviews the results for batch approval and regulatory compliance.

4. Accountability

The QC Manager is accountable for ensuring the HPLC testing is conducted in compliance with this SOP. The QA Manager is responsible for reviewing the results and approving the batch for release.

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5. Procedure

5.1 Sample Collection

  1. Collect a representative sample of tablets from the batch, as specified in the batch record.
  2. The sample should consist of a minimum of 6 tablets, or as specified in the batch record or pharmacopeial guidelines.
  3. Ensure that the tablets are free from defects such as cracks, chips, or contamination.
  4. Label the sample appropriately for identification during testing.

5.2 Preparation of Sample and HPLC Equipment

  1. Ensure the HPLC equipment is clean, calibrated, and ready for use.
  2. Set the HPLC system according to the specified method, ensuring the appropriate mobile phase, column, and detector settings as outlined in the batch record.
  3. Weigh the required amount of tablets (typically 10–20 tablets) and crush them to a fine powder.
  4. Weigh an appropriate amount of the powdered tablets for dissolution in a suitable solvent, such as methanol or water, depending on the solubility of the drug.
  5. Prepare the sample solution, ensuring that the tablet content is completely dissolved and filtered to remove any insoluble particles.

5.3 Calibration of HPLC System

  1. Prepare a calibration standard solution by dissolving a known quantity of the API in a solvent to create a standard concentration.
  2. Inject the standard solution into the HPLC system and record the chromatogram. Ensure that the retention time of the API matches the expected value for that particular method.
  3. Plot a calibration curve using the standard concentrations and their respective peak areas or heights. Ensure that the linearity is acceptable (typically R² > 0.99).

5.4 Performing HPLC Testing

  1. Inject the prepared sample solution into the HPLC system.
  2. Record the chromatogram and compare the retention time of the sample with that of the standard.
  3. Quantify the drug content by calculating the area of the API peak in the chromatogram and comparing it with the calibration curve generated from the standard solution.
  4. Ensure the API content falls within the specified range (usually 95%–105% of label claim) as outlined in the batch record or pharmacopeial guidelines.
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5.5 Data Recording and Calculation

  1. Record the results, including peak area, retention time, and the calculated concentration of the API, in the batch record (Annexure-1).
  2. Calculate the percentage of the drug content using the following formula:
    • % Drug Content = (Calculated Concentration / Label Claim Concentration) × 100
  3. Ensure that the calculated drug content meets the acceptance criteria for uniformity.

5.6 Acceptance Criteria

  1. The drug content should be within the acceptable limits specified in the batch record or pharmacopeial guidelines (typically ±5% of the label claim).
  2. If the drug content falls outside the acceptable range, investigate and document the findings in the deviation report (Annexure-2).
  3. Take corrective actions as necessary and perform re-testing if required.

5.7 Documentation and Record-Keeping

  1. Document all test results, including chromatograms, calculations, and observations, in the batch record (Annexure-1).
  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 all chromatograms, calibration curves, and raw data for future reference and audits.
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5.8 Post-Test Cleanup

  1. Clean all HPLC equipment, including syringes, injection ports, and sample vials, according to the cleaning SOP to prevent contamination between tests.
  2. Ensure the HPLC system is properly maintained and calibrated for future use.

6. Abbreviations

  • SOP: Standard Operating Procedure
  • GMP: Good Manufacturing Practice
  • QC: Quality Control
  • QA: Quality Assurance
  • API: Active Pharmaceutical Ingredient
  • HPLC: High-Performance Liquid Chromatography
  • RSD: Relative Standard Deviation

7. Documents

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

8. References

  • USP <621> – Chromatography
  • 21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals (US FDA)
  • European Pharmacopoeia (EP) – HPLC Testing

9. SOP Version

Version: 2.0

10. Approval Section

Prepared By Checked By Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Batch Record

Batch Number Tablet Sample Sample Weight (g) API Content (%) Result
Batch 001 Tablet Sample 0.5 99.2% Pass

Annexure-2: Deviation Report

Deviation Date Batch Number Deviation Description Corrective Action Responsible Person
15/12/2025 Batch 001 API content out of specification Reworked formulation and adjusted mixing process Jane Doe

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 Testing Procedures Refined HPLC testing protocols QA Head
Tablet Manufacturing V2.0 Tags:, , , , , , , , , , , , , , , , , , , , , , , , , ,