Standard Operating Procedure for Wet Granulation Equipment Setup and Operation
| Department | Tablet |
|---|---|
| SOP No. | SOP/TAB/002/2025 |
| Supersedes | SOP/TAB/002/2022 |
| Page No. | Page 1 of 10 |
| Issue Date | 20/02/2025 |
| Effective Date | 25/02/2025 |
| Review Date | 20/02/2026 |
1. Purpose
To establish a standardized, GMP-compliant method for setting up and operating the wet granulation equipment, ensuring optimal granule formation and product quality.
2. Scope
This SOP applies to the setup, calibration, and operation of the wet granulation equipment used in the tablet manufacturing process. It covers the preparation and granulation of active pharmaceutical ingredients (APIs) and excipients using wet methods.
3. Responsibilities
- Manufacturing Personnel: Set up and operate wet granulation equipment, monitor the process, and ensure correct material handling.
- Quality Control (QC): Ensure granulation meets specifications, monitor in-process quality, and perform equipment checks.
- Quality Assurance (QA): Oversee compliance with SOP and GMP guidelines and approve operational procedures.
4. Accountability
The Production Manager is responsible for ensuring the proper setup and operation of the wet granulation equipment. The QA Manager ensures the equipment meets compliance standards and approves operational procedures.
5. Procedure
5.1 Equipment Inspection and Preparation
- Inspect all components of the wet granulation equipment, including the granulator, mixer, spray system, and drying system, to ensure they are clean and functioning correctly.
- Verify that the equipment is free of residues from previous batches. Clean and sanitize all parts that will come into contact with the materials to prevent cross-contamination.
- Check the calibration status of all instruments, including the spray system, temperature controls, and moisture analyzers, and document the calibration dates.
5.2 Material Preparation
- Ensure that all materials for granulation, including active ingredients, excipients, and binder solution, are available and meet the specifications.
- Verify the identity, batch number, and certification of all incoming raw materials (e.g., Certificate of Analysis, Safety Data Sheets).
- Weigh and prepare the appropriate quantities of materials according to the batch formulation sheet.
- Prepare the binder solution, ensuring it is mixed to the correct concentration and is free from impurities.
5.3 Granulation Setup
- Load the dry powder blend (API and excipients) into the granulator, ensuring uniform distribution of all ingredients.
- Start the equipment and adjust the mixing parameters, including speed and duration, according to the formulation requirements.
- Slowly add the binder solution to the dry mixture while the equipment is running. Ensure the binder is evenly distributed to form a wet mass.
- Monitor the granulation process, adjusting the addition of binder and mixing speed as necessary to achieve the desired granule consistency and size.
5.4 In-Process Monitoring
- Monitor the temperature, humidity, and moisture content of the granulating mass throughout the process.
- Perform regular checks for uniformity of the wet granules, ensuring they meet the size and consistency specifications.
- If necessary, adjust the binder flow rate or granulation time to maintain uniform granule size and avoid over-wetting.
5.5 Granule Drying
- Once granulation is complete, transfer the granules to the drying system.
- Set the drying parameters (e.g., temperature, airflow) to ensure that the granules dry to the desired moisture content.
- Regularly monitor the drying process by checking moisture levels at intervals using a moisture analyzer. Ensure that the moisture content meets the required specification.
5.6 Equipment Shutdown and Cleaning
- After the granulation and drying process is complete, turn off the equipment and document the completion of the batch in the equipment log.
- Clean and sanitize all parts of the wet granulation equipment that came into contact with the raw materials, following the approved cleaning procedure.
- Inspect the equipment again after cleaning to ensure no residues remain and that all parts are in good working condition for the next batch.
5.7 Documentation and Record-Keeping
- Document all setup, operational, and cleaning activities in the batch record, including material lot numbers, equipment settings, and any deviations.
- Record all in-process quality checks, including moisture content, granule size, and equipment calibration results in the QC log (Annexure-1).
- Ensure that all records are signed by the responsible personnel and stored as per regulatory requirements for future audits and reference.
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
- Wet Granulation Equipment Setup Log (Annexure-1)
- Granulation Batch Record (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: Wet Granulation Equipment Setup Log
| Date | Equipment ID | Calibration Status | Operator | Comments |
|---|---|---|---|---|
| 20/02/2025 | Granulator 001 | Calibrated | John Doe | No issues |
| 21/02/2025 | Granulator 002 | Not Calibrated | Jane Smith | Calibration due next month |
Annexure-2: Granulation Batch Record
| Batch Number | Material Name | Binder Solution | Granulation Parameters | Test Results | Remarks |
|---|---|---|---|---|---|
| Batch 001 | Material A | Starch Solution | Mixing Time: 30 mins, Speed: 250 rpm | Moisture: 4.5%, Size Distribution: 80% < 500 µm | Within Specifications |
| Batch 002 | Material B | PVP Solution | Mixing Time: 40 mins, Speed: 300 rpm | Moisture: 5.2%, Size Distribution: 75% < 500 µm | Minor Deviations |
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 Setup Parameters | Standardization of Wet Granulation Process | QA Head |