This course is designed to give participants an understanding of the requirements for qualification of a lyophilizer and validation of lyophilization processes. Since lyophilizer sterilization and sterilization of the nitrogen system used to backfill require separate validation, media fills should primarily validate the filling, . With Lyophilizers and Freeze Dryer validation, it is essential to verify that the system can meet and control to the different temperature.

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The bulk of water removed from the product during freeze drying is via sublimation of all of the free ice crystals during the primary drying step. The usual number of temperature measuring points during process monitoring could be as high as one sensor placed in a representative sample vial or tray per shelf. Get the latest articles from Pharmaceutical Online delivered to your inbox. The measured product temperature will be colder than the shelf temperature set point during active primary drying because the heat from the shelf is being used for the sublimation phase change.

Depending on the application, moisture content in fully dried products is typically between 0. The collapse temperature of amorphous products is typically a few degrees warmer than its glass transition temperature. In addition to providing an extended shelf-life, successful freeze-drying should yield a product that has a short reconstitution time with acceptable potency levels.

Validation of Lyophilization

During the PQ replicate what was done during the original process validation. As freeze drying is a rather expensive process most products being processed are within the pharmaceutical and biotechnology industries. Purified Water System PQ. Additional primary drying endpoint determination tools are available on lyopbilizer freeze dryers equipped with advanced process control systems.

Certain products with high resistance to vapor flow in the dried portion of the cake may require that the shelf temperature be reduced towards the end of primary drying to keep the product temperature at its target and to avoid lyophioizer.


The purpose of the condenser is to attract the vapors being sublimed off of the product. The chamber is supplied with clean steam for sterilization. Frozen products can be categorized as either crystalline or amorphous glass in structure. She then joined Regeneron Pharmaceuticals in as Director, Manufacturing, being responsible for commercial manufacturing.

You need to break down the tasks, as trying to handle them all in one document would be messy and difficult. In session two of the three part series Lyophilization Validation: SP Scientific associates and distributors look forward to helping you reach your goals.

In addition to the free ice that is sublimed during primary drying, there remains a substantial avlidation of water molecules that are bound to the product. Another tool is available with freeze dryer designs that have external condensers.

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Harbour Group is a privately owned, operations focused company based in St. This removes the water content from product by a process called sublimation. It is extremely important that the sample be fully and completely frozen prior to pulling a vacuum and starting the drying process. Make sure production validagion a product process acceptance criteria. Condenser cooling rates are for information only.

More advanced shelf freeze dryers have freezing capability built into the product shelf which allows the product freezing to be accomplished inside the freeze dryer. However, certain complex biological products may actually become too dry for optimum storage results and the secondary drying process should be controlled accordingly.

A capacitance manometer always gives a true pressure reading in the product chamber. Session 2 of 3 Part Series: During annealing, the product temperature is cycled for example: With little control over heat flow into the product, it is more difficult to control the process. It is necessary to keep the product temperature safely below this critical temperature during primary drying to avoid collapse. Historically, validation of the lyophilization process focused on demonstrating three consecutive successful batches conducted in the commercial scale manufacturing operation.


In this VP, document how and why you are separating and scoping tasks.

After that time, no refunds will be approved. This valve can be closed for a short period of time and the subsequent rise in pressure in the product chamber can be measured. Organic solvents are also removed during primary drying. 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.

Freeze dryer refrigeration designs are available to provide the lower shelf and condenser temperatures needed vslidation freeze and then condense some organic solvents. The live transmission of data from all loggers placed inside of a chamber provides trouble free setup displaying accurate and instant valieation control along with documentation.

Session 2 of 3 Part Series: Lyophilization Process Validation – Part 1 – SP Scientific

About Our Trusted Brands. Part 1 – Process Validation Print Share. During primary drying, the system pressure and the shelf temperature are set and controlled in combination to yield the appropriate product temperature.

Three successful, consecutive, runs are performed. Sounds silly, but so often they lyophilise through a cycle and do not test or inspect.

The vacuum system consists of a separate vacuum pump connected to an airtight condenser and attached product chamber. When the super-cooled liquid finally freezes, it happens extremely quickly resulting in smaller ice crystals.

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