Standard Operating Procedure for Intermediate Precision Testing for Tablets
| Department | Quality Control |
|---|---|
| SOP No. | SOP/TAB/111/2025 |
| Supersedes | SOP/TAB/111/2022 |
| 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 intermediate precision testing of analytical methods for tablets, ensuring that the method is consistent and reproducible under different operational conditions.
2. Scope
This SOP applies to intermediate precision testing of analytical methods used for tablet formulations, including methods like HPLC, UV-Vis spectroscopy, and GC. It ensures that the testing process yields consistent results when conducted by different operators and at different times.
3. Responsibilities
- Quality Control (QC): Responsible for performing intermediate precision testing and ensuring that the method meets the required precision specifications.
- Quality Assurance (QA): Ensures that intermediate precision testing is performed according to the SOP and reviews the results for compliance with regulatory standards.
- Laboratory Personnel: Responsible for conducting intermediate precision testing, ensuring consistency in the results, and maintaining proper documentation.
4. Accountability
The QC Manager is accountable for ensuring that intermediate precision testing is performed accurately and in compliance with regulatory requirements. The QA Manager is responsible for reviewing and approving the results to ensure consistency and reliability.
5. Procedure
5.1 Test Preparation
- Review the analytical method to be tested for intermediate precision (e.g., HPLC, UV-Vis, or GC).
- Obtain a representative sample of the tablet formulation for testing.
- Prepare the sample and solutions as per the analytical method’s requirements.
- Ensure that the laboratory equipment and instruments (e.g., HPLC system, UV-Vis spectrophotometer) are calibrated and functioning properly before starting the tests.
5.2 Selection of Operators
- Choose at least two qualified laboratory personnel who will perform the testing independently to ensure operator variability.
- Ensure that both operators are trained in the same method and use the same procedure for testing, but perform the tests at different times and possibly under different conditions (e.g., different equipment setups, different shifts).
5.3 Intermediate Precision Testing Procedure
- Perform the analysis for the tablet sample using the selected analytical method (e.g., HPLC, UV-Vis, or GC) according to the method’s standard operating procedure.
- Have each operator conduct the analysis at separate times to account for variability in the method. Ensure that the same set of samples and conditions is used for each test.
- Each operator should perform multiple replicate tests (usually 6–10) per condition to assess precision.
- Record all relevant data, including sample preparation, instrument settings, and results of the analysis.
5.4 Data Analysis
- Calculate the mean, standard deviation, and coefficient of variation (CV) for the results obtained by each operator.
- Compare the variability between the two operators. The data should be evaluated using the following criteria:
- The CV for each operator should not exceed a predefined limit (usually 2%–5%, depending on the method and specifications).
- The difference in mean results between operators should be minimal, indicating consistency.
- If the CV for either operator exceeds the predefined limit, further investigation should be carried out to determine the cause of the inconsistency.
5.5 Acceptance Criteria
- The analytical method is considered to have passed the intermediate precision test if the variation between the results from both operators is within the acceptable limits (e.g., CV <5%).
- If the test results do not meet the acceptance criteria, investigate the reasons for the failure and perform corrective actions (e.g., retraining of operators, equipment maintenance, or recalibration).
5.6 Documentation and Record-Keeping
- Document all intermediate precision testing results, including the data from each operator, statistical calculations, and any deviations from the expected results in the batch record (Annexure-2).
- Ensure that all records are signed, dated, and stored according to the company’s record retention policy for future audits and inspections.
- Maintain raw data, including chromatograms, spectra, and test reports, for regulatory compliance and future reference.
5.7 Post-Test Actions
- Clean the laboratory equipment and instruments after each use to avoid cross-contamination between tests.
- Dispose of any used samples, reagents, or solvents according to the company’s waste disposal procedures.
- Ensure that the analytical instruments are regularly calibrated and maintained according to the manufacturer’s instructions and company SOPs.
6. Abbreviations
- SOP: Standard Operating Procedure
- GMP: Good Manufacturing Practice
- QC: Quality Control
- QA: Quality Assurance
- CV: Coefficient of Variation
- HPLC: High-Performance Liquid Chromatography
- UV-Vis: Ultraviolet-Visible Spectroscopy
- GC: Gas Chromatography
7. Documents
- Batch Record (Annexure-2)
- Deviation Report (Annexure-1)
8. References
- USP <621> – Chromatography
- 21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals (US FDA)
- European Pharmacopoeia (EP) – Specifications for Chromatography and Method Validation
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 | High variability in operator results | Retrained operators and recalibrated equipment | John Doe |
Annexure-2: Batch Record
| Batch Number | Operator 1 Result | Operator 2 Result | Mean Result | CV (%) | Pass/Fail |
|---|---|---|---|---|---|
| Batch 001 | 98.0% | 97.8% | 97.9% | 0.2% | 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 Data Analysis Method | Improved method consistency | QA Head |