Tarelli E, Elphick A D, Gostick J D, Stammers R P
Division of Chemistry, National Institute for Biological Standards and Control, Potters Bar, Herts, UK.
J Biol Stand. 1987 Oct;15(4):331-40. doi: 10.1016/s0092-1157(87)80006-9.
Aqueous solutions of the carbohydrates alpha alpha'-trehalose, mannitol and lactose, human serum and human albumin were freeze-dried in ampoules and part of each batch was further desiccated over phosphorus pentoxide in a manner similar to that used to prepare international biological standards and related materials. The residual moisture present in the preparations and their uptake of moisture was then measured by Karl Fischer titration. In ampoules open to atmosphere [22 degrees C, 34% relative humidity (RH)] freeze-dried serum, albumin, lactose and alpha alpha'-trehalose all exhibited hygroscopic properties, their moisture contents rising over a period of 24 h, to 10%, 8%, 8% and 7%, respectively. Mannitol when dried to low moisture levels did not exhibit hygroscopic properties, but the residual moisture in different freeze-dried batches was very variable, possibly as a result of that solid's sponge-like and/or crystalline microstructure. When exposed to the same conditions, dried materials in ampoules fitted with polythene capillary leak plugs (used routinely at this Institute during the preparation of Biological Standards) exhibited a considerably reduced rate of moisture uptake. The effect of secondary vacuum drying over phosphorus pentoxide on the moisture content of these preparations is also reported.
将碳水化合物α,α'-海藻糖、甘露醇和乳糖的水溶液、人血清与人白蛋白在安瓿中进行冷冻干燥,每一批次的一部分再以类似于制备国际生物标准品及相关材料的方式在五氧化二磷上进一步干燥。然后通过卡尔费休滴定法测定制剂中存在的残留水分及其吸湿量。在暴露于大气环境(22摄氏度,34%相对湿度(RH))的安瓿中,冷冻干燥的血清、白蛋白、乳糖和α,α'-海藻糖均表现出吸湿性,其水分含量在24小时内分别升至10%、8%、8%和7%。甘露醇干燥至低水分含量时未表现出吸湿性,但不同冷冻干燥批次中的残留水分变化很大,这可能是由于该固体呈海绵状和/或晶体微观结构所致。当暴露于相同条件时,装有聚乙烯毛细管泄漏塞(本研究所在制备生物标准品时常规使用)的安瓿中的干燥材料吸湿速率显著降低。还报告了在五氧化二磷上进行二次真空干燥对这些制剂水分含量的影响。