Standard Operating Procedure for Dry Granulation Method for Tablets
| Department | Tablet |
|---|---|
| SOP No. | SOP/TAB/003/2025 |
| Supersedes | SOP/TAB/003/2022 |
| Page No. | Page 1 of 10 |
| Issue Date | 25/02/2025 |
| Effective Date | 01/03/2025 |
| Review Date | 25/02/2026 |
1. Purpose
To define the procedure for the dry granulation method in tablet manufacturing, ensuring uniformity, integrity, and compliance with GMP standards.
2. Scope
This SOP applies to the dry granulation process for tablet production, including powder blending, compaction, and granule processing.
3. Responsibilities
- Manufacturing Personnel: Operate the dry granulation equipment, monitor the process, and ensure material handling is correct.
- Quality Control (QC): Perform in-process checks and verify that the granules meet the required specifications.
- Quality Assurance (QA): Ensure compliance with SOP, GMP standards, and regulatory requirements.
4. Accountability
The Production Manager is responsible for ensuring the correct operation of the dry granulation method. The QA Manager ensures adherence to SOPs and regulatory compliance.
5. Procedure
5.1 Equipment Inspection and Setup
- Inspect all dry granulation equipment, including the roller compactor, mills, and sieves, to ensure cleanliness and proper working order.
- Ensure that all components are free from contaminants and have been cleaned according to the cleaning SOP.
- Check calibration of all measurement instruments such as the weight scales and compaction pressure gauge.
5.2 Material Preparation
- Verify all raw materials, including active pharmaceutical ingredients (APIs) and excipients, for compliance with specifications (e.g., Certificates of Analysis, batch numbers).
- Weigh all materials according to the formulation requirements, ensuring that the proportions align with the approved batch formula.
- Ensure that the materials are free-flowing and do not require additional powder blending before the granulation process.
5.3 Dry Granulation Process
- Load the pre-weighed material into the roller compactor.
- Set the appropriate compaction force based on the material specifications to form the compacted ribbons.
- Ensure uniformity of ribbon thickness and appearance. If ribbons are not uniform, adjust the equipment settings (e.g., roller gap, force) accordingly.
- Once the ribbons are formed, feed them into the mill to break them into smaller granules of the desired size.
- Monitor the granule size distribution using a sieve or particle size analyzer. Adjust milling conditions if the size does not meet the required specification.
5.4 In-Process Monitoring
- Regularly monitor the granulation process, checking parameters such as compaction pressure, ribbon quality, and granule size.
- Document all in-process parameters, including compaction pressure, roller speed, and granule size.
- Verify that the moisture content of the granules remains within the acceptable limits to prevent clumping or uneven compaction.
5.5 Final Quality Control
- Once the granules have been produced, perform quality control tests on granule uniformity, size distribution, and moisture content.
- If the granules do not meet the specifications, evaluate potential adjustments to the equipment settings or material formulation.
- Document all testing results and any corrective actions taken in the batch records.
5.6 Equipment Shutdown and Cleaning
- After the granulation process, power off the equipment and disconnect from the main power supply.
- Perform a thorough cleaning of the granulation equipment, including the rollers, mills, and sieves, using the approved cleaning SOP.
- Inspect the equipment post-cleaning to ensure all parts are free of residues and ready for the next batch.
5.7 Documentation and Record-Keeping
- Record all operational steps, including material used, equipment settings, and any deviations or adjustments made during the process in the batch record.
- Document all quality control results (granule size, moisture content, etc.) in the QC Log (Annexure-1).
- Ensure all records are reviewed, signed, and stored according to regulatory requirements for traceability and audits.
6. Abbreviations
- SOP: Standard Operating Procedure
- API: Active Pharmaceutical Ingredient
- GMP: Good Manufacturing Practice
- QC: Quality Control
- QA: Quality Assurance
- CoA: Certificate of Analysis
7. Documents
- Dry Granulation Batch Record (Annexure-1)
- Granule Quality Control Log (Annexure-2)
8. References
- 21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals (US FDA)
- EU GMP Guidelines Part I – Basic Requirements for Medicinal Products
- ICH Q7 – Good Manufacturing Practice Guide for Active Pharmaceutical Ingredients
9. SOP Version
Version: 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | |||
| Designation | |||
| Department |
11. Annexures
Annexure-1: Dry Granulation Batch Record
| Batch Number | Material Name | Granulation Parameters | Granule Size | Moisture Content | Remarks |
|---|---|---|---|---|---|
| Batch 001 | Material A | Compaction Pressure: 50 kN, Speed: 25 rpm | 75% < 500 µm | 4.5% | Within specifications |
| Batch 002 | Material B | Compaction Pressure: 55 kN, Speed: 28 rpm | 78% < 500 µm | 5.2% | Minor adjustments needed |
Annexure-2: Granule Quality Control Log
| Batch Number | Test Performed | Result | Test Date | QC Personnel |
|---|---|---|---|---|
| Batch 001 | Particle Size | Pass | 25/02/2025 | John Doe |
| Batch 002 | Moisture Content | Pass | 26/02/2025 | Jane Smith |
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 Granulation Parameters | Standardization of Dry Granulation Process | QA Head |