In Situ Determination of the Physical State of Biological Samples during Freeze Drying

Abstract

The proceeding change of water content in a freeze-drying process, as well as the physical state of cell–sugar suspensions with Lactobacillus paracasei ssp. paracasei, was monitored by means of an in situ weighing system. Due to the pressure and temperature variations in the drying chamber, the weighing system was found to be influenced. This deviation of the weighing system was quantified by means of drying simulations with drying-inert Teflon dummies. This quantified deviation could be used for correction of the following freeze-drying processes. The applicability of this correction method was verified by drying model sugar solutions with known dry matter. Taking the quantified drift of the balance into account, the measured water contents for the model solution were proved to deviate less than 5% from the actual value. Finally, this verified correction method was applied to freeze drying of cell–sugar suspensions. As a result, the drying course of the cell–sugar samples could be depicted in the appropriate state diagram. Thus, the weighing system could be used to monitor the state transitions, which the bacterial suspension experienced during freeze drying, and qualified for specific investigations on the glassy state during freeze drying.

Keywords:

• Freeze drying
• Glassy state
• In situ measurement
• Physical state
• Residual water content

ACKNOWLEDGMENTS

This work was supported by Deutsche Forschungsgemeinschaft (DFG) Project Reference: KU 750/2-1.