新型直链淀粉手性固定相反相拆分烯唑醇对映体  

Enantiomeric Separation of Diniconazole by New Type of Amylose Chiral Stationary Phase

作　　者：王雪松[1,2] 徐浩[2] 王祥云[2] 章虎[2] 王新全[2] 

机构地区：[1]东北农业大学农学院,哈尔滨150030 [2]浙江省农业科学院农产品质量标准研究所,杭州310021

出　　处：《农药》2011年第10期711-713,共3页Agrochemicals

基　　金：国家自然科学基金资助项目(20807038);浙江省农科院科技创新提升工程(2007R19Y01E02)

摘　　要：[目的]采用新型直链淀粉-三（5-氯-2-甲基苯基氨基甲酸酯）涂敷型手性固定相在反相色谱条件下拆分烯唑醇对映体。【方法】利用高效液相色谱-手性固定相法考察流动相组成及温度对手性拆分的影响，对烯唑醇对映体进行了旋光测定。[结果]烯唑醇在直链淀粉-三（5-氯-2-甲基苯基氨基甲酸酯）手性固定相上为（-）-对映体先出峰；烯唑醇对映体在所考察的流动相组成（乙腈含量100％-30％）及温度（5-45℃）范围内均未能达到基线分离。[结论]（-）-（R）-烯唑醇先于其对映体被洗脱；实验烯唑醇对映体分离的最佳流动相配比为乙腈-水（体积比30：70），最佳分离温度为25℃；基于线性Van·t Hoff曲线的热力学参数证明对映体的分离受焓影响。[Aims] Enantiomeric separation of diniconazole was evaluated under reversed-phase high-performance liquid chromatography with new amylose-tris（5-chlorine-2-methylphenylcarbamate） chiral stationary phase. [Methods] Highperformance liquid chromatography which coupled with amylose-tris（5-chlorine-2-methylphenylcarbamate） chiral stationary phase was used. Elution order of enantiomers was determined by polarimetric detector. The effects of different mobile phase compositions and temperature of column on the chiral separation were investigated. [Results] The result showed that the （-）-diniconazole was eluted firstly through amylose-tris（5-chlorine-2-methylphenylcarbamate） chiral stationary phase. Base line separation was not achieved under any composition of mobile phase with the content of acetonitrile range from 100 to 30% as well as the temperature range from 5 to 45 ℃. [Conclusions] （-）-（R）-diniconazole was eluted firstly; in terms of retention time and column pressure, best enantiomeric separation of diniconazole achieved with acetonitrile and water（30：70, by vol） and the optimized temperature was 25 ℃. Thermodynamical parameters illustrated that enantiomeric separation of diniconazole was driven by enthalpy.

关 键 词：直链淀粉-三(5-氯-2-甲基苯基氨基甲酸酯)手性固定相 烯唑醇对映体 反相色谱 

分 类 号：TQ450.1[化学工程—农药化工]