Bergren M S, Chao R S, Meulman P A, Sarver R W, Lyster M A, Havens J L, Hawley M
Pharmacia and Upjohn Inc., Kalamazoo, MI 49001, USA.
J Pharm Sci. 1996 Aug;85(8):834-41. doi: 10.1021/js9600078.
Delavirdine mesylate was recrystallized from solution under a variety of conditions. Seven crystal forms and a stable amorphous phase were isolated from solution. Two of these crystal forms were polymorphic anhydrates: from XI (U-90152T) and form VIII (U-90152S). Two hydrates (forms VI and XIV), an ethanol solvate (form VII), an acetonitrile solvate (form XIII), and a solvate from methanol/acetone (from XII) were also identified. Six additional phases were identified as the products of solid-state transformations of the hydrated and solvated phases. The solid phases were differentiated by infrared spectroscopy and X-ray powder diffraction. Several of the solid-state phase transformations were mediated by atmospheric moisture. These transformations were studied as a function of relative humidity with dynamic moisture sorption gravimetry (DMSG). DMSG also provided useful measurements of hygroscopicity.
甲磺酸地拉韦啶在多种条件下从溶液中重结晶。从溶液中分离出了七种晶型和一种稳定的非晶相。其中两种晶型为多晶型无水物：晶型XI（U - 90152T）和晶型VIII（U - 90152S）。还鉴定出两种水合物（晶型VI和XIV）、一种乙醇溶剂化物（晶型VII）、一种乙腈溶剂化物（晶型XIII）以及一种甲醇/丙酮溶剂化物（晶型XII）。另外六个物相被鉴定为水合相和溶剂化相固态转变的产物。通过红外光谱和X射线粉末衍射对固相进行区分。一些固态相变是由大气湿度介导的。利用动态水分吸附重量法（DMSG）研究了这些转变与相对湿度的关系。DMSG还提供了有用的吸湿性测量数据。
