氯霉素类药物的高效液相色谱手性分离研究  

Study of Chiral Separation of Chloramphenicol Analogs by High Performance Liquid Chromatography

作　　者：何红梅[1] 徐秀珠[1] 潘春秀[1] 沈报春[1] 张雪君[1] 

机构地区：[1]浙江大学化学系,杭州310027

出　　处：《分析化学》2005年第2期165-168,共4页Chinese Journal of Analytical Chemistry

基　　金：浙江省分析测试基金资助项目(No.03111)

摘　　要：利用Pirkle型(S,S) Whelk O1手性柱对合霉素、甲砜霉素、氟甲砜霉素进行了对映体分离研究。考 察了在正己烷流动相中醇类添加剂种类及浓度对其手性分离的影响,并采用液相色谱/质谱联用法对甲砜霉 素的两个异构体峰进行了确证。结果表明:当异丙醇和叔丁醇为醇类添加剂时,合霉素和甲砜霉素获得较大 分离因子,而使得氟甲砜霉素获得较大分离因子的是乙醇。合霉素在流动相为正己烷/乙醇=97∶3时获得最 大分离度是1.89;在正己烷/乙醇=90∶10时,甲砜霉素、氟甲砜霉素都获得了很好的分离,最佳分离度Rs分 别达到1.84和3.94。The Whelk-O1 chiral stationary phase (CSP) is a valuable column for the high performance liquid chromatography ( HPLC) resolution of the enantiomers of a wide variety of compounds. So the resolution of enantiomers of three compounds, which are the synthomycin and the thiamphenicol (THA) and the florfenicol (FLR), were studied on (S,S)-Whelk-O1 CSP using HPLC using n-hexane and alcohol additives as mobile phase. And the influence of the type and concentration of alcohol additives on chiral separation of solutes was investigated. Then the enantiomers of THA were confirmed by liquid chromatography-mass speatrometry The results showed that three compounds were separated successfully. When iso-propanol and tert-butanol as mobile-phase additives, the separation factor (a) of synthomycin and THA was higher in contrast to ethanol. However, ethanol was more favorable for chiral separation of FLR. Furthermore, the best resolution of synthomycin was 1.89 using a mobile-phase of n-hexane/ethanol (97:3), and that of THA and FLR was separately 1.84 and 3.94 when a mobile-phase of n-hexane/ethanol (90: 10) was used. So the method which was used to separate the enantiomers of this type of drugs was got and was also used to determinate the single isomer content which was about 0.5% in the drug as an impurity.

关 键 词：甲砜霉素 正己烷 乙醇 药物 高效液相色谱 手性分离 氯霉素类 联用法 手性柱 醇类 

分 类 号：TQ465[化学工程—制药化工]