Standard Operating Procedure for Operating Lyophilizers for Nasal Powders
1) Purpose
This SOP outlines the procedures for operating lyophilizers to produce nasal powder formulations. Lyophilization, or freeze-drying, ensures that moisture is removed from nasal powders, preserving the product’s stability and shelf life.
2) Scope
This SOP applies to all personnel involved in the operation and maintenance of lyophilizers used for nasal powder production at [Company Name].
3) Responsibilities
- Operators: Responsible for setting up and operating the lyophilizer according to product specifications and batch requirements.
- Quality Assurance (QA): Ensures that the lyophilized powders meet the required moisture content and stability specifications.
- Maintenance Team: Ensures the lyophilizer is functional and calibrated for accurate temperature and vacuum control.
4) Procedure
4.1 Pre-Operation Setup
4.1.1 Inspection of Lyophilizer
- Visually inspect the lyophilizer to ensure that it has been properly cleaned and is free of any residues from previous batches. Verify that all seals, gaskets, and connections are secure.
- Document the pre-operation inspection in the equipment log.
4.1.2 Setup Parameters
- Set the lyophilizer parameters, including freezing temperature, primary drying temperature, secondary drying temperature, and vacuum level, according to the
formulation’s requirements. Record the settings in the Batch Manufacturing Record (BMR).
Ensure that the product trays are correctly loaded and spaced for efficient heat transfer.
4.2 Operation of the Lyophilizer
4.2.1 Freeze-Drying Process
- Start the freeze-drying cycle by freezing the product at the specified freezing temperature. Monitor the chamber temperature to ensure that the product is frozen uniformly.
- Once the product is completely frozen, initiate the primary drying phase by reducing the chamber pressure to the required vacuum level and gradually raising the shelf temperature to sublimate the frozen water.
- Continue the primary drying process until the majority of the water has been removed, then transition to the secondary drying phase to remove any remaining bound water.
4.2.2 In-Process Checks
- Perform regular checks on the product’s moisture content and temperature during the freeze-drying cycle. Record the moisture content in the in-process testing log.
- Adjust the drying parameters if necessary to achieve the desired moisture content. Record any adjustments in the BMR.
4.3 Post-Operation Activities
4.3.1 Shutdown Procedure
- After the freeze-drying cycle is complete, stop the vacuum and return the chamber to atmospheric pressure. Open the chamber and carefully remove the lyophilized product trays.
- Turn off the lyophilizer and allow the unit to cool down before cleaning or performing maintenance.
4.3.2 Cleaning of Lyophilizer
- Disassemble any removable parts and clean all components with an approved cleaning solution. Rinse thoroughly with sterile water and allow to air dry or use lint-free wipes.
- Document the cleaning process in the cleaning log and submit for QA review before the next operation.
4.4 Maintenance of Lyophilizer
4.4.1 Routine Maintenance
- Inspect the lyophilizer weekly for wear and tear on critical components such as vacuum pumps and heat transfer plates. Perform any necessary repairs or replacements as needed.
- Record all maintenance activities in the maintenance log.
4.4.2 Annual Calibration
- Calibrate the lyophilizer’s temperature control and vacuum systems annually to ensure accurate freeze-drying performance. Document calibration results in the calibration log.
5) Abbreviations, if any
- BMR: Batch Manufacturing Record
- QA: Quality Assurance
6) Documents, if any
- Batch Manufacturing Record (BMR)
- In-Process Testing Log
- Cleaning Log
- Maintenance Log
- Calibration Log
7) References, if any
- Manufacturer’s lyophilizer manual
- Internal SOP for cleaning and maintenance
8) SOP Version
Version 1.0
Annexure
1. In-Process Testing Log Template
| Date | Batch No. | Moisture Content (%) | Temperature (°C) | Operator Initials | QA Approval |
|---|---|---|---|---|---|
| DD/MM/YYYY | Batch Number | Moisture Content Measured | Temperature Measured | Operator Name | QA Name |