高速逆流色谱-重结晶法制备高纯度三尖杉宁碱和紫杉醇  

Preparation of high purity cephalomannine and taxol with high speed countercurrent chromatography and recrystallization

作　　者：林楠[1] 王尉[1] 高峡[1,2] 张经华 

机构地区：[1]北京市理化分析测试中心有机材料检测技术与质量评价北京市重点实验室,北京100089 [2]北京市食品安全分析测试工程技术研究中心,北京100089

出　　处：《分析仪器》2018年第1期184-189,共6页Analytical Instrumentation

基　　金：北京市财政资金项目(PXM2016_178305_000017)资助

摘　　要：通过高效液相色谱测定紫杉醇粗提物中三尖杉宁碱和紫杉醇的纯度分别为33.1%和36.5%,采用正己烷-醋酸乙酯-甲醇-乙醇-水(5∶7∶5∶1∶6.5,v/v)体系,利用高速逆流色谱仪分离得到三尖杉宁碱和紫杉醇馏出物纯度分别为88.4%和89.7%,以50%乙腈进行重结晶后,三尖杉宁碱和紫杉醇纯度分别为98.7%和97.6%。The purities of cephalomannine and taxol in their crude extracts were 33.1% and 36.5% ,respectively,determined by high performance liquid chromatography（HPLC）.Then the above cephalomannine and taxol were further separated by high speed countercurrent chromatography with n-hexanemethanol-ethanol-water-acetic acid ethyl ester（5∶7∶5∶1∶6.5,vd/v）mobile phase,and their purity were 88.4% and 89.7% ,respectively.Finally,the purified cephalomannine and taxol were recrystallized with 50% acetonitrile and their purities were up to 98.7% and 97.6% ,respectively.

关 键 词：高速逆流色谱 重结晶 三尖杉宁碱 紫杉醇 

分 类 号：O657.72[理学—分析化学] TQ464[理学—化学]