(S)-与(R)-五味子丙素的HPLC手性分离及质谱研究  

Separation and Study of (S)-and(R)-Schizandrin C by HPLC and Mass Spectrometry with Chiral Derivatization

作　　者：董黎红[1] 李岩峰[2] 郭晓河[1] 王强[3] 常俊标[1,3] 

机构地区：[1]河南省分析测试中心,河南郑州450002 [2]天津大学药物科学与技术学院,天津300072 [3]郑州大学化学系,河南郑州450001

出　　处：《分析测试学报》2009年第8期931-934,939,共5页Journal of Instrumental Analysis

基　　金：国家杰出青年科学基金资助项目(30825043)

摘　　要：建立了一种反相高效液相色谱法分析(S)-和(R)-五味子丙素对映异构体的方法。选用Chiralcel OD-RH手性色谱柱,以甲醇和水(体积比78∶22、97∶3)为流动相,流速0.5 mL/min,254 nm波长下检测,五味子丙素合成中间体噁唑啉取代联苯对映异构体2和2的保留时间分别为22.2 min和19.9 min,分离度为2.5,五味子丙素对映异构体3和3的保留时间分别为7.5、9.0 min,与相邻杂质峰分离度分别为3.2和2.7。经液相色谱-质谱实现了分离与鉴定。方法灵敏度高、重复性好,可用于五味子丙素对映异构体的立体选择性研究及质量控制。A reserved-phase high performance liquid chromatography （RP-HPLC） method was developed for separation of enantiomers of （S）- and （R）- schizandrin C. The experimental conditions were optimized. The result indicated that the enantiomers was successfully separated on a Chiralcel OD-RH column by using MeOH- H2O（78 ： 22, 97 ： 3, by volume） as mobile phase with flow rate of 0. 5 mL/min at 254 nm. The retention time of（dioxazoline-biphenyl） enantiomers 2＇ and 2 were 19.9, 22.2 rain, respectively, with resolution factor of 2.5. And the retention time of schizandri C enantiomers 3＇ and 3 were 7.5 and 9.0 min, respectively, their resolution factors were 3.2, 2.7 with the adjacent impurity, respectively. The separation and identification of （S）-and （R）- schizandrin C were carried out by LC -MS. The method was reproducible and sensitive, and could be applied in the structural study and quality evaluation of schizandrin C enantiomers.

关 键 词：五味子丙素 液相色谱-质谱 手性柱 对映异构体分离 

分 类 号：O657.63[理学—分析化学]