Standard Operating Procedure for Vacuum Drying Procedure in API Manufacturing
| Department | API Manufacturing |
|---|---|
| SOP No. | SOP/API/065/2025 |
| Supersedes | SOP/API/065/2022 |
| Page No. | Page 1 of 10 |
| Issue Date | 13/04/2025 |
| Effective Date | 15/04/2025 |
| Review Date | 13/04/2026 |
1. Purpose
To establish a standard and validated procedure for drying active pharmaceutical ingredients (APIs) and intermediates using vacuum drying to remove moisture or solvents under controlled low-pressure conditions, ensuring product quality, stability, and GMP compliance.
2. Scope
This SOP applies to all vacuum drying operations conducted in tray-type or rotary vacuum dryers within the API manufacturing facility. It covers loading, operation, monitoring, unloading, and cleaning activities.
3. Responsibilities
- Production Operator: Perform vacuum drying as per batch record and monitor critical parameters.
- Production Supervisor: Ensure proper equipment usage, record review, and verification of completeness.
- QA Department: Review BMR and drying logs for compliance.
- Engineering Team: Maintain dryer, vacuum pumps, and temperature control systems.
4. Accountability
The Production Head is accountable for the correct execution of vacuum drying operations. QA is responsible for final release based on documentation review.
5. Procedure
5.1 Pre-Drying Activities
- Verify line clearance for drying room is completed and recorded.
- Ensure:
- Dryer is clean and labeled appropriately
- Vacuum pump is operational
- All gauges, temperature controllers, and timers are functional
- Record pre-checks in the “Vacuum Dryer Equipment Checklist” (Annexure-1).
5.2 Tray Loading and Equipment Setup
- Transfer loaded trays from the previous step (see SOP/API/064/2025) and arrange them inside the dryer chamber.
- Ensure trays are arranged for maximum airflow and heat distribution.
- Close the chamber door securely and verify gasket tightness.
- Set:
- Drying temperature (e.g., 40–60°C or as per BMR)
- Vacuum level (e.g., -650 mmHg or specified)
- Drying time (as per batch record)
5.3 Drying Operation
- Start the vacuum pump and initiate heating cycle simultaneously.
- Monitor and record:
- Chamber temperature and jacket temperature
- Vacuum level every 30 minutes
- Any abnormal noise, vapor leakage, or odor
- Sample material at defined intervals to check moisture content (LOD or Karl Fischer method).
- Document drying observations in the “Vacuum Drying Log” (Annexure-2).
5.4 Completion and Unloading
- Upon achieving desired moisture level, stop heating and allow to cool under vacuum.
- Break vacuum slowly and open dryer chamber.
- Collect dried material in clean, labeled SS containers.
- Record unloading time, product weight, and observations.
5.5 Post-Drying Activities
- Clean dryer as per cleaning SOP and update cleaning log.
- Record total drying yield and reconcile with issued material.
- Submit samples to QC for final analysis.
6. Abbreviations
- SOP: Standard Operating Procedure
- LOD: Loss on Drying
- QC: Quality Control
- QA: Quality Assurance
- SS: Stainless Steel
- BMR: Batch Manufacturing Record
7. Documents
- Vacuum Dryer Equipment Checklist (Annexure-1)
- Vacuum Drying Log (Annexure-2)
- Batch Manufacturing Record
8. References
- ICH Q7 – Good Manufacturing Practice for Active Pharmaceutical Ingredients
- WHO TRS 1019 – Annex 2
- Internal Process Validation Protocols
9. SOP Version
Version: 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | |||
| Designation | |||
| Department |
11. Annexures
Annexure-1: Vacuum Dryer Equipment Checklist
| Date | Dryer ID | Vacuum Pump Status | Door Seal Status | Heater Function | Remarks |
|---|---|---|---|---|---|
| 13/04/2025 | VD-01 | OK | OK | OK |
Annexure-2: Vacuum Drying Log
| Date | Batch No. | Start Time | End Time | Temp (°C) | Vacuum (mmHg) | LOD (%) | Operator |
|---|---|---|---|---|---|---|---|
| 13/04/2025 | API-DRY-20250413 | 08:30 | 14:00 | 50 | 660 | 0.28 |
Revision History:
| Revision Date | Revision No. | Details | Reason | Approved By |
|---|---|---|---|---|
| 01/01/2022 | 1.0 | Initial SOP Release | Process Control | QA Head |
| 13/04/2025 | 2.0 | Enhanced Monitoring, Annexures Added | Regulatory Audit Compliance | QA Head |