Standard Operating Procedure for In-Process Particle Size Distribution Testing
| Department | Tablet |
|---|---|
| SOP No. | SOP/TAB/146/2025 |
| Supersedes | SOP/TAB/146/2022 |
| Page No. | Page 1 of 6 |
| Issue Date | 01/03/2026 |
| Effective Date | 06/03/2026 |
| Review Date | 01/03/2027 |
1. Purpose
To define the procedure for testing the particle size distribution of granules or powders during the tablet manufacturing process to ensure the product meets the required quality standards for uniformity and performance.
2. Scope
This SOP applies to the in-process monitoring of particle size distribution during tablet granulation, blending, and final tablet formation to ensure consistent tablet quality and dissolution properties.
3. Responsibilities
- Quality Control (QC): Responsible for conducting the particle size distribution tests on granules or powders during various stages of tablet production.
- Production Operator: Responsible for sampling the material at specified intervals and ensuring the sample is representative for testing.
- Quality Assurance (QA): Ensures compliance with this SOP and reviews particle size distribution data to confirm that it meets specifications.
4. Accountability
The QC Manager is accountable for ensuring that particle size distribution tests are performed at appropriate stages of tablet production. The QA Manager ensures that the process is followed, and that the results are reviewed and approved in accordance with quality standards.
5. Procedure
5.1 Sampling
- During granulation and blending stages, collect samples of granules or powders at defined intervals (e.g., every 100 kg or after each batch of granulation).
- Ensure the sample is representative of the entire batch and is collected following the sampling procedure outlined in the relevant SOP.
5.2 Preparing Testing Equipment
- Ensure the particle size analyzer or sieve shaker is clean and calibrated according to the manufacturer’s instructions and internal calibration procedures.
- Prepare the equipment and set it up to match the type of material being tested (e.g., dry sieving, laser diffraction).
5.3 Performing Particle Size Distribution Testing
- Weigh a sufficient amount of the sample to meet the requirements of the particle size testing method (typically 10-50 grams depending on the material).
- Test the sample using the appropriate method (e.g., laser diffraction, sieve analysis). Follow the method’s specific instructions regarding time and procedure.
- Record the particle size distribution results, including the d50, d90, and any other relevant parameters as specified in the product specifications.
5.4 Documentation and Records
- Document the particle size distribution data in the batch record (Annexure-2), including the sample number, test method, and results.
- If any deviations are observed from the acceptable particle size distribution range, generate a deviation report (Annexure-1) and initiate an investigation into the cause of the deviation.
5.5 Acceptance Criteria
- The particle size distribution of the granules or powders must fall within the predefined specifications to ensure consistent tablet performance, including dissolution rate and tablet uniformity.
- If the results fall outside the specified range, corrective actions must be taken, and the batch may need to be rejected or reprocessed.
5.6 Post-Testing Actions
- If the particle size distribution meets the specifications, proceed with the next stages of tablet production, such as compression or coating.
- If the particle size is out of specification, review the process, investigate the root cause, and take corrective actions such as rework or formulation adjustments.
6. Abbreviations
- SOP: Standard Operating Procedure
- GMP: Good Manufacturing Practice
- QC: Quality Control
- QA: Quality Assurance
- d50: Median particle size
- d90: Particle size at 90% cumulative distribution
7. Documents
- Batch Record (Annexure-2)
- Deviation Report (Annexure-1)
8. References
- USP <701> – Granulation and Particle Size Testing
- 21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals (US FDA)
- European Pharmacopoeia (EP) – Particle Size Distribution Specifications
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 | Particle size exceeded acceptable range | Reprocessed batch and adjusted granulation process | John Doe |
Annexure-2: Batch Record
| Sample Number | Particle Size Distribution | Action Taken |
|---|---|---|
| Sample 1 | 90% < 200 μm | Accepted |
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 | Added in-process testing requirements | Process improvement | QA Head |