摘要
针对异山梨醇高效液相色谱保留时间为17~18min时产生的杂质进行了研究。首先通过减压蒸馏和结晶等方式对异山梨醇产品进行后处理。当减压精馏切除前馏分为30%时,该杂质可去除。乙酸乙酯结晶除杂效果更佳。其次对异山梨醇产品进行液质联用检测,并结合相关文献对检测结果进行分析,初步断定杂质结构和该杂质产生原因。最后提出在生产过程中控制该杂质的方法。
The impurity produced by isosorbide which was showed at a retention time of 17-18min in high performance liquid chromatography(HPLC)were studied in this paper.Firstly,isosorbide products were reprocessed by vacuum distillation and crystallization.The impurity could be removed when the front cut fraction was removed 30%.Recrystallization in acetic ester was better for impurity removing.Secondly,isosorbide products were tested by LC-MS,and the test results were analyzed in combination with the relevant literature,so as to preliminarily determine the impurity structure and the reason why the impurity produced.Finally,a method to control the impurity in the production process was proposed.
作者
张满满
束长月
曹智敏
Zhang Man-man;Shu Chang-yue;Cao Zhi-min
出处
《化工设计通讯》
CAS
2020年第5期158-159,共2页
Chemical Engineering Design Communications
关键词
异山梨醇
杂质
提纯
isosorbide
impurity
purification
