Drying of an active pharmaceutical ingredient, in the form of a crystalline hydrate, was investigated using a small-scale flow cell methodology. A new laboratory tool was developed and demonstrated using a simple segregated column technique to quickly distinguish different drying mechanisms using a minimal number of experiments. For the case studied here, increasing vacuum levels improved the removal of solvents while use of nitrogen flow through the solids facilitated water removal. Additional results are presented from experiments conducted to assess the impact of the crystallization solvent system and washing on drying behavior and cake properties. A system was identified which avoided issues associated with poor cake handling and improved overall drying performance. This article provides details on the new experimental method used that helped lead to the rapid development of an improved drying process and presents results demonstrated through the pilot plant scale.

中文翻译：

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阐明活性药物成分干燥机制的新小规模方法

使用小规模流动池方法研究了结晶水合物形式的活性药物成分的干燥。使用简单的分离柱技术开发并演示了一种新的实验室工具，可以通过最少的实验快速区分不同的干燥机制。对于此处研究的案例，增加真空水平改善了溶剂的去除，而使用氮气流过固体则促进了水的去除。为评估结晶溶剂系统和洗涤对干燥行为和滤饼性质的影响而进行的实验提供了额外的结果。确定了一种系统，该系统可以避免与滤饼处理不良相关的问题，并提高整体干燥性能。