Standard Operating Procedure for Sampling Granules from Fluidized Bed Process
| Department | Tablet |
|---|---|
| SOP No. | SOP/TAB/154/2025 |
| Supersedes | SOP/TAB/154/2022 |
| 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 sampling granules during the fluidized bed granulation process to ensure the granules meet quality standards and specifications before further processing.
2. Scope
This SOP applies to the sampling of granules produced in the fluidized bed process, ensuring uniformity in the granules’ size, moisture content, and other physical properties before proceeding with tablet compression or coating.
3. Responsibilities
- Quality Control (QC): Responsible for performing the sampling procedure, ensuring that samples are representative and testing them for granule quality parameters.
- Granulation Operator: Responsible for ensuring that the granulation process is conducted as per the SOP and assisting QC with the sampling of granules.
- Quality Assurance (QA): Ensures that the sampling process is compliant with the SOP and reviews the results for consistency with the product specifications.
4. Accountability
The QC Manager is accountable for ensuring that the granules are sampled at the correct times and in a manner that ensures accurate and representative testing. The QA Manager ensures that all steps of the process are followed correctly and approves the test results.
5. Procedure
5.1 Preparation for Sampling
- Ensure that the sampling tools, such as clean sampling equipment, gloves, and containers, are prepared and ready for use.
- Verify that the fluidized bed system is operating within the defined parameters for granulation, including airflow, temperature, and humidity.
- Ensure that the sampling area is clean and appropriately designated for the sampling process.
5.2 Granule Sampling Method
- Granules must be sampled from different points within the fluidized bed system to ensure that the sample is representative of the entire batch.
- Sample granules from the top, middle, and bottom sections of the fluidized bed. At least three separate points should be sampled to get a homogeneous sample.
- If the fluidized bed is equipped with an automatic sampling system, ensure that the system is calibrated and functioning properly. Otherwise, manual sampling should be performed at the specified intervals.
5.3 Sample Size
- Sample a minimum of 1-2 kg of granules from each selected point (or as per the batch size and sampling plan).
- The total sample size should be representative of the batch and adequate for further testing, such as moisture content, particle size distribution, and uniformity.
5.4 Sampling Interval
- Samples should be taken at predefined intervals during the granulation process (e.g., every 30 minutes or as specified by the production batch parameters).
- Ensure that samples are taken before any further processing steps, such as drying, to maintain the accuracy of the sample’s characteristics.
5.5 Documentation of Sample Collection
- Document the sampling process in the batch record (Annexure-2), including the sample number, sampling point, date, time, and operator details.
- Record the number of samples collected and any relevant observations regarding the granulation process.
5.6 Analysis of Granules
- Perform the necessary analyses on the samples, including moisture content, particle size distribution, and uniformity testing.
- Document the results of the analysis in the batch record, noting any deviations from the predefined specifications.
5.7 Corrective Actions
- If the granules do not meet the quality specifications, initiate corrective actions such as adjusting the granulation parameters (e.g., drying time, temperature) or modifying the formulation.
- Re-sample and analyze the granules after corrective actions have been implemented to confirm that the issue has been resolved.
5.8 Post-Sampling Actions
- After successful sampling and analysis, proceed with the next stage of tablet manufacturing, such as drying or compression.
- If issues persist, initiate a thorough review of the granulation process and make any necessary adjustments before continuing production.
6. Abbreviations
- SOP: Standard Operating Procedure
- GMP: Good Manufacturing Practice
- QC: Quality Control
- QA: Quality Assurance
- Moisture Content: The percentage of water present in the granules
- Particle Size Distribution: The distribution of particle sizes in the granules
7. Documents
- Batch Record (Annexure-2)
- Deviation Report (Annexure-1)
8. References
- USP <701> – Granulation and Moisture Testing for Tablets
- 21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals (US FDA)
- European Pharmacopoeia (EP) – Guidelines for Granulation and Tablet Production
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 | Moisture content outside acceptable range | Adjusted drying time and recalibrated equipment | John Doe |
Annexure-2: Batch Record
| Sample Number | Moisture Content | Particle Size Distribution | Uniformity Test Result | Action Taken |
|---|---|---|---|---|
| Sample 1 | 3.5% | Pass | Pass | 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 | Updated granule sampling criteria | Improved process accuracy | QA Head |