Characterization techniques: The stepping stone to liposome lyophilized product development

The primary drying is the longest step of the freeze-drying process and becomes one of the focuses for lyophilization cycle development inevitably, which is often approaching through a "trial and error" course and requires a labor-intensive and time-consuming endeavor. Nevertheless, drawing support from characterization techniques to understand the physic-chemical properties changing of the sample during lyophilization and their correlation with process conditions comprehensively, the freeze-drying development and optimization will get more from less. To get the optimal lyophilization cycle in the least time, the instrumental methods assisting primary drying design are summarized. The techniques used for estimating the collapse temperature of products are reviewed at first, aiming to provide a reference on the primary drying temperature setting to guarantee product quality. The instrumental methods for primary drying end prediction are also discussed to get optimal freeze-drying protocol with higher productivity. This review highlights the practicality of the above techniques through expounding basic principles, typical measurement conditions, merits and drawbacks, interpretation of results and practical applications, etc. At last, the techniques used for residual moisture detection of lyophilized products and size determination after liposome rehydration are briefly introduced.