反相色谱条件下三唑类手性农药对映异构体的拆分  

Chiral Resolution of Eight Triazole Pestioioles by High Performance Liquid Chromatography Under Reversed Phase Conditions

作　　者：田芹[1] 任丽萍[2] 吕春光[3] 周志强[3] 

机构地区：[1]国家地质实验测试中心,北京100037 [2]中国农业大学动物科技学院,北京100094 [3]中国农业大学理学院应用化学系,北京100094

出　　处：《分析化学》2010年第5期688-692,共5页Chinese Journal of Analytical Chemistry

基　　金：自然科学基金(No.20777093)资助项目

摘　　要：采用自制的纤维素-三(3,5-二甲基苯基氨基甲酸酯)手性固定相(CDMPC-CSP)和直链淀粉-三(3,5-二甲基苯基氨基甲酸酯)手性固定相(ADMPC-CSP),在反相色谱条件下成功地拆分了己唑醇、烯唑醇、烯效唑、粉唑醇、三唑酮和戊唑醇对映异构体。考察了固定相类型、不同比例的甲醇/水或乙腈/水做流动相、柱温等因素对三唑类手性农药拆分的影响,优化了色谱分离的条件。结果表明:两种固定相都有很强的拆分能力。在优化的色谱条件下,己唑醇和烯唑醇在这两种固定相上都能被分离;三唑酮只能在CDMPC-CSP上分离;粉唑醇、戊唑醇、烯效唑只能在ADMPC-CSP上分离。流动相中水的含量增加会使对映体的保留增强,分离的可能性增大。在0～40℃研究温度范围内,容量因子k随温度的升高而减少,除烯效唑与戊唑醇外,其它手性农药的选择因子α也随温度的升高而减少,而分离度Rs随温度变化没有明显的规律,最好的分离度不都出现在低温。对映体流出顺序用圆二色检测器测定。The chiral resolutions of the racemic pesticides, hexaconazole, diniconazole, uniconazole, flutriafol, tebuconazole and triadimefon were successfully carried out using cellulose（tris-3,5-dimethyl-phenylcarbamate）（CDMPC） and amylose（tris-3,5-dimethylphenyl-carbamate, ADMPC） as chiral stationary phases by high performance liquid chromatography under reversed phase conditions. The influences of the chiral stationary phases（CSPs）, methanol/water or acetonitrile/water of the different ratios as the mobile phases and temperature on chiral resolutions were investigated and the chromatographic conditions were optimized. The results showed that the two CSPs exhibited high chiral recognition ability in reversed-phase HPLC and methanol, acetonitrile and water content in mobile phases affected the enantiomeric resolutions and retentions. Hexaconazole and diniconazole were separated on both CSPs. Triadimefon was separated only on the CDMPC-CSP. Uniconazole, flutriafol and tebuconazole were separated only on the ADMPC-CSPs. The retention factors（k） and selectivity factor（α） for the enantiomers of most investigated pesticides decreased with the increase of temperature except for those of tebuconazole and uniconazole in methanol/water. Better resolutions were not always at low temperature. The elution orders of the eluting enatiomers were determined by a circular dichrism（CD） detector.

关 键 词：三唑类手性农药 手性拆分 反相色谱 手性固定相 

分 类 号：TQ450.1[化学工程—农药化工]