Standard Operating Procedure for High-Pressure Homogenization Analysis for Coated Tablets
| Department | Quality Control |
|---|---|
| SOP No. | SOP/TAB/117/2025 |
| Supersedes | SOP/TAB/117/2022 |
| 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 conducting high-pressure homogenization analysis of coated tablets, ensuring uniform distribution of active pharmaceutical ingredients (APIs) and excipients within the tablet coating.
2. Scope
This SOP applies to the testing of tablet coatings subjected to high-pressure homogenization processes. The procedure assesses the uniformity of the coating, ensuring consistency in the API distribution, thickness, and performance of the coating during tablet manufacturing.
3. Responsibilities
- Quality Control (QC): Responsible for performing high-pressure homogenization testing, ensuring uniform distribution of coating materials and APIs within the tablets.
- Quality Assurance (QA): Ensures the analysis is conducted according to this SOP and reviews results to confirm compliance with product specifications and regulatory guidelines.
- Laboratory Personnel: Responsible for preparing the sample, performing the homogenization analysis, and recording the results.
4. Accountability
The QC Manager is accountable for ensuring that high-pressure homogenization analysis is performed accurately and consistently, adhering to quality standards. The QA Manager is responsible for reviewing and approving results to ensure that the product complies with the necessary regulatory and internal requirements.
5. Procedure
5.1 Sample Preparation
- Obtain a representative batch of coated tablets to be tested.
- If testing coated tablets, ensure that they are free from damage and defects such as chips or cracks in the coating.
- Prepare the sample by crushing the tablets gently, ensuring uniform powder distribution, if required, for analysis.
- Weigh an appropriate amount of the tablet powder for homogenization testing (usually 100 mg or more depending on the protocol).
5.2 Setting Up High-Pressure Homogenization
- Ensure the homogenizer is set to the appropriate pressure range for tablet coating analysis (typically 500-2000 bar, depending on the coating material).
- Fill the homogenization chamber with the prepared tablet sample.
- Adjust the homogenizer settings for the required cycle time and pressure based on the tablet formulation.
- Check that the homogenizer is properly calibrated before starting the analysis to ensure accurate results.
5.3 Performing Homogenization Analysis
- Run the homogenization process for the selected number of cycles to ensure uniform distribution of the coating material within the tablet matrix.
- Record the pressure, temperature, and cycle time used for the process for each sample.
- After completion, collect a small sample of the homogenized coating and tablet powder for analysis.
5.4 Particle Size Distribution and Coating Thickness Measurement
- Perform particle size distribution analysis on the homogenized sample using appropriate equipment, such as laser diffraction or sieve analysis.
- Measure the coating thickness of a few representative tablets using a micrometer or optical microscopy. Record the results in a detailed report.
- Ensure the coating thickness and particle size distribution fall within the acceptable range, typically ensuring a consistent and uniform coating.
5.5 Data Analysis and Evaluation
- Analyze the data to evaluate the uniformity of the coating, API distribution, and particle size range. The coating should exhibit minimal variation within the sample.
- If the results show excessive variation or deviations from the expected particle size or coating thickness, investigate the cause of inconsistency.
- Document the results and compare them to the predefined specifications. The analysis should show a consistent and uniform coating without agglomeration or particle size abnormalities.
5.6 Acceptance Criteria
- The coated tablets should have uniform particle size distribution with minimal deviation between individual tablets.
- The coating thickness should be within the acceptable range specified in the product’s formulation guidelines (typically ±10% of the target thickness).
- If the results do not meet the acceptance criteria, initiate corrective actions, such as adjusting the homogenization parameters or modifying the coating process.
5.7 Documentation and Record-Keeping
- Record all high-pressure homogenization analysis results, including cycle conditions, particle size distribution, and coating thickness data, in the batch record (Annexure-2).
- Ensure all records are signed, dated, and stored in accordance with the company’s record retention policy.
- Maintain raw data, including chromatograms, particle size analysis results, and any deviation reports, for regulatory compliance and future reference.
5.8 Post-Test Actions
- Clean the homogenizer and associated equipment after each use to remove any residual sample material and prevent cross-contamination.
- Dispose of used tablet samples and solvents according to the company’s waste disposal procedures.
- Ensure that the homogenizer is regularly serviced and calibrated according to the manufacturer’s guidelines and company SOPs.
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
- SEM: Scanning Electron Microscopy
7. Documents
- Batch Record (Annexure-2)
- Deviation Report (Annexure-1)
8. References
- USP <1161> – Granulation and Coating Techniques
- 21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals (US FDA)
- European Pharmacopoeia (EP) – Stability Testing and Coating Standards
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 | Inconsistent particle size in coating | Adjusted homogenizer settings and re-tested | John Doe |
Annexure-2: Batch Record
| Batch Number | Sample Weight (g) | Homogenization Pressure (bar) | Particle Size (µm) | Coating Thickness (µm) | Result |
|---|---|---|---|---|---|
| Batch 001 | 100 g | 1500 bar | 150 µm | 25 µm | 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 homogenization pressure limits | Improved testing conditions | QA Head |