Lyophilization or freeze drying is a process in which water is removed from a product after it is frozen and placed under a vacuum, allowing the ice to change. For composing validation protocol of lyophilizer need to carry out its qualification test and. decide acceptance criteria. So during selection of. Hi all, I have a question regarding an OQ of a freeze dryer. Im Validation Manager in a medium size medical devices company and have the.

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Hydrocarbon levels on swabs should not exceed the negative control. If you have one that is excellent.

When the super-cooled liquid finally freezes, it happens extremely quickly resulting in smaller ice crystals. The condenser temperature required is dictated by the freezing point and collapse temperature of the product. The vacuum system consists of a separate vacuum pump connected to an airtight condenser and attached luophilizer chamber. Manifold freeze dryers rely on ambient conditions to provide the heat of sublimation to the product.

Larger ice crystals improve the speed of the freeze drying process because of the larger vapor pathways left behind in the dried portion of the product as the ice crystals are sublimated.

At the end of primary drying when all of the free ice crystals qualificattion been sublimed, the product will appear to be dried. Since all of the free ice has been removed in primary drying, the product temperature can now be increased considerably without fear of melting or collapse.

Condenser Capacity Loss of weight from a weighed lyophillzer of water in trays is not less than the stated capacity of the condenser. View recent webinars on ” Techniques for Enhancing Visualization of Lyophilization Cakes “; the three-part series on ” Lyophilization Validation: Similarly, if bulk drying, the area around the thermocouple wire will dry more quickly than other areas in the product tray. In addition to defrosting the condenser and cleaning the system after each cycle, routine freeze dryer maintenance typically includes periodic changing of vacuum pump oil and visually checking all seals and gaskets.

  ISO 20765 PDF

Validation equipment recommended for Autoclaves, Sterilizers and ovens. Determination of the critical collapse lyophklizer of a product is an important step in establishing and optimizing a freeze drying process. Because the condenser is maintained at a lower energy level relative to the product ice, the vapors condense and turn back into solid form ice in the condenser. The Vacuum System is tested by determining the blank-off pressure, pump ultimate pressure and leak-up rate.


Harbour Group is a privately owned, operations focused company based in St. The Pirani gauge, however, will give a false high reading in the presence of water vapor.

This is the water that is removed desorbed during secondary drying. Without knowing the critical temperature of the product, a trial and error approach is required to determine appropriate primary drying temperatures.

It is best not to freeze a large qualificstion of sample in the bottom of a flask because the sample will be too thick for efficient water removal.

Operation Qualification for Lyophilization

Freeze drying is the removal of ice or other frozen solvents from a material through the process of sublimation and the removal of bound water molecules through the process of desorption. Because product will dry from the top down, the tip of the thermocouple should always be placed at the very bottom and center of the container.


We’ll assume you’re ok with that, but you can opt-out if you wish. Lyophilized products are extremely hydroscopic and they must be sealed in air tight containers following freeze drying to prevent rehydration from atmospheric exposure.

Product trays with removable-bottoms are available when working with vials. The purpose of the condenser is to attract the vapors being sublimed off of the product. All vials are stoppered No vials are damaged. All three methods of heat transfer – conduction, convection and radiation, must be considered when freeze drying a product.


Organic solvents are also lyolhilizer during primary drying. Also, the flask might break due to uneven stress. Shelf freeze dryers allow the precise control of cooling rates which affects product freezing rates and crystal size. In a clean room environment with very few particulates for ice nucleation, there is a significantly greater amount of super-cooling. Request a Quote Interested in learning more about our products?

When sublimation of ice crystals is complete, the product temperature will increase and approach the shelf temperature.

A recommended approach is to first set the system pressure using the vapor pressure of ice table. Performance Qualification Acceptance Criteria Sterilization Bacillus stearothermophilus biological indicators are such that the product of the ‘D’ value and the log of the population is at least 6 e.