SOP Guide for Pharma

Tablets: SOP for Analytical Method Validation for Tablets – V 2.0

Auditor

Tablets: SOP for Analytical Method Validation for Tablets – V 2.0

Standard Operating Procedure for Analytical Method Validation for Tablets

Department Tablet
SOP No. SOP/TAB/091/2025
Supersedes SOP/TAB/091/2022
Page No. Page 1 of 8
Issue Date 01/03/2026
Effective Date 06/03/2026
Review Date 01/03/2027

1. Purpose

To define the procedure for validating analytical methods used to determine the quality, potency, and purity of tablets, ensuring that these methods are accurate, precise, and reproducible.

2. Scope

This SOP applies to the validation of all analytical methods used in the testing of tablets, including but not limited to assay, dissolution, content uniformity, and impurity testing.

3. Responsibilities

4. Accountability

The QC Manager is accountable for ensuring that the method validation is conducted in compliance with this SOP and for reporting the results. The QA Manager is responsible for reviewing the method validation results and approving the method for routine testing.

5. Procedure

5.1 Method Development

  1. Identify the analytical method to be validated, such as HPLC, UV spectrophotometry, or dissolution testing, as required by the product specifications.
  2. Develop the method based on the required parameters, considering sample preparation, instrument calibration, and detection limits.
  3. Ensure that the method is capable of detecting the required analytes, such as the active pharmaceutical ingredient (API) or impurities, in the expected concentration ranges.
See also  Tablets: SOP for Calibration of Fluid Bed Processor for Granulation - V 2.0

5.2 Validation Protocol Preparation

  1. Prepare a validation protocol outlining the following details:
    • Scope and objective of validation
    • Test methods to be validated
    • Acceptance criteria for accuracy, precision, specificity, linearity, range, and robustness
    • Sample preparation procedure
    • Testing equipment and conditions
  2. Ensure the validation protocol is reviewed and approved by QA before testing begins.

5.3 Validation Testing

  1. Conduct validation tests based on the protocol, ensuring that the method meets the following criteria:
    • Accuracy: The method’s ability to measure the true value of the analyte. Perform recovery studies using spiked samples and calculate the percentage recovery.
    • Precision: The repeatability and reproducibility of the method. Perform repeatability tests (intra-day and inter-day) and calculate the %RSD (Relative Standard Deviation).
    • Specificity: The ability of the method to measure the analyte in the presence of other substances, such as excipients or degradation products. Perform interference studies to demonstrate specificity.
    • Linearity: The ability of the method to produce results that are directly proportional to the concentration of the analyte. Perform a calibration curve and determine the correlation coefficient (R²).
    • Range: The concentration range over which the method is accurate and precise. Perform tests at various concentrations within the method’s expected range.
    • Robustness: The ability of the method to remain unaffected by small variations in operational parameters (e.g., temperature, pH). Perform stress testing and document the results.
  2. Document all raw data, including chromatograms, calculations, and observations, in the validation report (Annexure-1).
See also  Tablets: SOP for Wet Granulation Equipment Setup and Operation - V 2.0

5.4 Data Evaluation

  1. Evaluate the data obtained from the validation tests to ensure that the method meets the acceptance criteria specified in the validation protocol.
  2. Calculate the precision, accuracy, linearity, and other validation parameters, and compare them against the established criteria.
  3. If any test does not meet the specified acceptance criteria, identify the cause of failure, document the findings, and take corrective actions as necessary.

5.5 Approval of Method

  1. If the analytical method meets all the acceptance criteria, prepare a validation report summarizing the results and conclusions (Annexure-2).
  2. Submit the validation report to QA for review and approval.
  3. If the method fails any of the criteria, initiate an investigation, document the findings, and revalidate the method if necessary.

5.6 Documentation and Record-Keeping

  1. Ensure that all method validation activities are documented, including test results, observations, calculations, and any corrective actions taken in the validation report (Annexure-2).
  2. Store the validation report, raw data, and all relevant documentation in the company’s records management system for future reference and audits.
  3. Ensure that all records are signed, dated, and retained in accordance with the company’s record retention policy.

5.7 Post-Validation Activities

  1. After the method is validated and approved, ensure that it is implemented in routine testing as per the standard operating procedures (SOPs).
  2. Periodically review the performance of the validated method through ongoing testing to ensure continued compliance with regulatory standards.
See also  Tablets: SOP for Using Fluidized Bed Processor in Tablet Manufacturing - V 2.0

6. Abbreviations

7. Documents

  1. Validation Protocol (Annexure-1)
  2. Validation Report (Annexure-2)

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: Validation Protocol

Test Method Acceptance Criteria Test Date Result Remarks
HPLC Assay ±2% of label claim 01/02/2026 Pass Method validated successfully

Annexure-2: Validation Report

Method Parameter Result Acceptance Criteria Comments
HPLC Assay Accuracy 99.5% ±2% Pass
HPLC Assay Precision 1.2% RSD ≤2% 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 Validation Protocol Refined validation methods QA Head
Exit mobile version