亚微米C18键合硅胶固定相加压毛细管电色谱法同时拆分3种手性三唑类农药  

Simultaneous chiral separation of three triazole pesticide enantiomers with submicron C18 bonded silica stationary phase by pressurized capillary electrochromatography

作　　者：陈巧梅[1] 柳青 申琳 薛芸[1] 王彦[1] 阎超[1] CHEN Qiaomei;LIU Qing;SHEN Lin;XUE Yun;WANG Yan;YAN Chao(School of Pharmacy,Shanghai Jiaotong University,Shanghai 200240,China)

机构地区：[1]上海交通大学药学院,上海200240

出　　处：《色谱》2018年第4期388-394,共7页Chinese Journal of Chromatography

基　　金：上海市科委科研计划项目(16142200300;17142201000);上海市引进技术的吸收与创新专项(XC-ZXSJ-02-2016-11);上海市标准化推进专项(17DZ2201500)~~

摘　　要：采用改良Stber法制备420 nm亚微米单分散二氧化硅微球,采用C18硅烷化修饰后装填成毛细管色谱柱。采用该色谱柱,在加压毛细管电色谱平台上成功地实现了3对手性三唑类农药烯效唑、烯唑醇和丙环唑的同时拆分和分离。考察了各因素对手性分离效果的影响,优化后的色谱条件为:流动相为乙腈-20 mmol/L磷酸盐缓冲液(pH=6.8)(45∶55,v/v),其中缓冲液中含20 mmol/L羟丙基-γ-环糊精(HP-γ-CD);泵流速为0.04 mL/min;施加电压-9.4 kV;检测波长220 nm。在上述条件下,烯效唑、烯唑醇和丙环唑3种对映体同时得到拆分和分离,相邻两峰之间的分离度依次为4.20、12.9、4.41、4.09、1.70,分离时间仅为12 min,柱效最高达到310 000 plates/m。该研究为手性三唑类农药的同时分离提供了新的分离分析思路。A monodispersed C18 silica stationary phase with particle size of 420 nm was prepared by modified Stober method.The column packed with submicron C18 bonded silica was successfully used for simultaneous enantioseparation of three chiral triazole pesticides by pressurized capillary electrochromatography(pCEC).Some effects on separation were investigated,and the optimized conditions were as follows:mobile phase of acetonitrile and 20 mmol/L phosphate buffer(pH=6.8)containing 20 mmol/L(2-hydroxypropyl)-γ-cyclodextrin(HP-γ-CD)(45∶55,v/v),flow rate of 0.04 mL/min and applied voltage of-9.4 kV,the detection wavelength at 220 nm.The resolutions of adjacent peaks of uniconazole,diniconazole and propiconazole enantiomers were 4.20,12.9,4.41,4.09 and 1.70 in 12 min,respectively,with the column efficiency up to 310 000 plates/m.This study provides an alternative way for the simultaneous separation of chiral triazole pesticides with high efficiency.

关 键 词：加压毛细管电色谱 亚微米二氧化硅微球 手性三唑类农药 手性流动相添加剂 羟丙基-γ-环糊精 

分 类 号：O658[理学—分析化学]