Standard Operating Procedure for Assay Method Validation for Enteric-Coated Tablets
| Department | Tablet |
|---|---|
| SOP No. | SOP/TAB/076/2025 |
| Supersedes | SOP/TAB/076/2022 |
| Page No. | Page 1 of 7 |
| Issue Date | 01/03/2026 |
| Effective Date | 06/03/2026 |
| Review Date | 01/03/2027 |
1. Purpose
To provide a standardized procedure for validating assay methods used for determining the active pharmaceutical ingredient (API) content in enteric-coated tablets.
2. Scope
This SOP applies to the validation of assay methods for enteric-coated tablets, ensuring accurate and reliable quantification of the API content in the tablets.
3. Responsibilities
- Manufacturing Personnel: Responsible for providing the required tablet samples for assay method validation and ensuring the samples are correctly identified and handled.
- Quality Control (QC): Responsible for performing the assay method validation, recording the results, and ensuring that the method meets the specified accuracy, precision, and other validation criteria.
- Quality Assurance (QA): Ensures that the assay method validation process is followed according to this SOP and reviews the results for final approval and batch release.
4. Accountability
The QC Manager is accountable for ensuring the assay method validation is performed in compliance with this SOP and reporting the results. The QA Manager is responsible for reviewing and approving the method validation results and approving the final batch for release.
5. Procedure
5.1 Preparation for Assay Method Validation
- Ensure that all necessary equipment, reagents, and solvents for the assay method are available and meet the required specifications.
- Verify that the equipment, including the HPLC system or any other relevant equipment, is calibrated and functioning properly according to the manufacturer’s specifications.
- Prepare the required concentrations of the API and any internal standards used in the method, ensuring that they are of known purity and accurately quantified.
5.2 Assay Method Validation Parameters
The following parameters must be validated for the assay method:
- Accuracy: Verify that the assay method provides results that are close to the true value. This is typically performed by testing a known concentration of the API and comparing the results with the expected values.
- Precision: Verify the method’s repeatability by performing multiple measurements of the same sample and calculating the standard deviation.
- Linearity: Test a series of API concentrations to ensure the assay method produces a linear response across the expected range of concentrations.
- Specificity: Verify that the method can accurately measure the API in the presence of excipients and other potential interfering substances.
- Limit of Detection (LOD) and Limit of Quantification (LOQ): Determine the lowest concentration of the API that can be reliably detected and quantified.
- Robustness: Assess the method’s resistance to small changes in the analytical conditions, such as temperature or pH.
5.3 Validation Execution
- Prepare calibration standards with known concentrations of the API and perform the assay using the validation method.
- Run the validation samples and record the results for each parameter.
- For each parameter, calculate the results and ensure they meet the predefined acceptance criteria set for accuracy, precision, linearity, specificity, LOD, LOQ, and robustness.
- Perform replicate testing to confirm precision and consistency of results.
5.4 Data Analysis and Reporting
- Analyze the data from the validation tests, ensuring that all results are within the acceptable limits specified in the batch record or pharmacopeial guidelines.
- Prepare a report summarizing the validation results, including the methodology, data, acceptance criteria, and conclusions about the validity of the assay method (Annexure-1).
- Document any deviations or failures from the acceptance criteria in the deviation report (Annexure-2) and initiate corrective actions if necessary.
5.5 Documentation and Record-Keeping
- Document all assay method validation results, including data for accuracy, precision, linearity, and other parameters in the validation report (Annexure-1).
- Record any deviations or failures from the validation criteria in the deviation report (Annexure-2), along with the corrective actions taken.
- Ensure that all records are signed, dated, and stored according to the company’s record retention policy for future audits and inspections.
5.6 Post-Validation Activities
- If the assay method passes validation, it may be used for routine analysis of enteric-coated tablets as part of the quality control process.
- If the assay method fails any validation criteria, investigate the cause, make the necessary adjustments to the method, and re-validate.
- Ensure that any changes to the assay method are documented and validated in accordance with this SOP.
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
7. Documents
- Batch Record (Annexure-1)
- Deviation Report (Annexure-2)
8. References
- USP <1225> – Validation of Compendial Methods
- 21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals (US FDA)
- ICH Q2(R1) – Validation of Analytical Procedures: Text and Methodology
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 Report
| Test Parameter | Specification | Result | Pass/Fail |
|---|---|---|---|
| Accuracy | ±2% | ±1.5% | Pass |
| Precision | ±2% | ±1.8% | Pass |
Annexure-2: Deviation Report
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You said: html Annexure-2: Deviation Report
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