1. Lyophilization Technology 03/2011

2. 03/03/2011Lyophilizer Tech. Summary | 03 March 20112 What is freeze-drying Why is it used A means of preservation Used to provide a stable product that may be stored for a long time. Applied to products and materials that may change if heat is applied. A dehydration process Involves sublimation A batch process and can take a long time.

3. 03/03/2011Lyophilizer Tech. Summary | 03 March 20113 Advantages of Lyophilization Proteins thermally sensitive can be dried. Products sensitive to oxygen can be sealed in N2. In a vial the fill volume is accurate giving better dosage control than powder filling. The second drying step can be controlled to give excellent long term storage properties. No change in moisture level during storage. More control of the environment compared with other methods. Products are more stable after lyophilizing.

4. 03/03/2011Lyophilizer Tech. Summary | 03 March 20114 What kind of products can be freeze-dried Non-biological products  heat-labile chemicals Non-living bio products (majority)  enzymes, hormones, antibiotics, vitamins, blood products, antibodies, vaccines, pharmaceuticals bone and body tissues for surgical/medical use, foodstuffs Living organisms Miscellaneous materials

5. 03/03/2011Lyophilizer Tech. Summary | 03 March 20115 Required from a lyophilized material? Dried to the right moisture content Ethically acceptable Cosmetically Refined Active! Stable Cake like Clean

6. 03/03/2011Lyophilizer Tech. Summary | 03 March 20116 Refrigeration Vacuum Systems Equipment Faultfinding Temperature Freeze Dryer Design Cycle Development Critical temperature Shelf temperature Product temperature Pre- Freezing stage Holding period Primary drying Secondary Drying Time

7. 03/03/2011Lyophilizer Tech. Summary | 03 March 20117 The Process for lyophilization 1.Solution preparation, Depth in a vial is 0.5 inch. The water based products are typically < 10% solutions. 2.Freezing, Freeze to -40 0 C. Freezing below a critical temperature before the drying process. Kept at its lowest temperature for a given period to ensure all the material is frozen. Form large, contiguous ice crystals. Be frozen quickly. Freeze rate is 1 0 C/minute 3.Primary Drying. Supply of heat and the pressure used. Involve Sublimation 4.Secondary Drying 5.Stoppering (vials) 6.Final condition

8. 03/03/2011Lyophilizer Tech. Summary | 03 March 20118 Sublimation  Solid (ice) to a vapor.  An energy intensive process  Latent heat of sublimation of ice 2800 kJ/kg (1200Btu/lb).  In Lyophilizing step, product must go from a solid form to a vapor.  For sublimation to occur, supply the energy.

9. 03/03/2011Lyophilizer Tech. Summary | 03 March 20119 Phase Diagram for Pure Water 760 torr 100 0 C 4 torr Liquid Triple point Vapor Solid Product Temp.

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