生物发酵制备骨化二醇相关杂质的分离及结构鉴定  

Preparation and Identification of the Related Impurities from Biotransfomated Calcifediol

作　　者：席章姣 翟龙飞[1] 谢洪兵[1] 曾志刚[1] 

机构地区：[1]成都大学四川抗菌素工业研究所,四川成都610052

出　　处：《精细化工》2014年第8期979-982,1023,共5页Fine Chemicals

基　　金：四川省科技厅技术市场及成果交易计划研究项目(2008CO0002);科技部"十二五"重大新药创制专项子项目(2011ZX09401-403-9)~~

摘　　要：生物发酵的骨化二醇发酵液经板框过滤,液液萃取以及高压制备色谱精制,得到色谱纯度为97.5%的骨化二醇相关杂质单体。通过紫外、质谱和核磁共振波谱综合解析,确证了杂质的化学结构为骨化二醇的同分异构体,即24-羟基维生素D3,是不同于化学合成的一个新的杂质。该实验中确定的制备条件可以为该杂质的制备提供参考,所得杂质单品可以为后续实验提供杂质对照品。An impurity existing in the production of calcifediol, with a purity of 97.5%, was obtained by frame filtering, liquid-liquid extraction and refined by high pressure preparative chromatography. The chemical structure of the impurity was confirmed by UV, MS and NMR, which proved that the impurity, named 24-hydroxy vitamin D3 , was a structural isomer of calcifediol. It was a new impurity different from the chemosynthesis. The preparation conditions were established by the experiment, which will provide references for the preparation of the impurity. The obtained impurity can be used as reference substance in the follow-up experiments.

关 键 词：骨化二醇 杂质 制备 结构鉴定 生物工程 

分 类 号：TQ466.4[化学工程—制药化工]