纤维素键合手性固定相拆分喹禾灵对映体  

Enantiomeric Resolution of Quizalofop-ethyl on Immobilized Cellulose Chiral Stationary Phase

作　　者：袁庆东[1] 沈国强[1] 张晓天[1] 江乾[1] 王保国[1] 张金利[1] 李韡[1] 

机构地区：[1]天津大学化工学院,天津300072

出　　处：《分析测试学报》2012年第12期1536-1539,共4页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(NSFC 20836005);教育部博士点基金资助项目

摘　　要：采用Chiralpak IC(纤维素-三(3,5-二氯苯基氨基甲酸酯)键合在5μm硅胶上)键合型手性柱,建立了喹禾灵对映体的高效液相色谱拆分方法。系统考察了流动相组成、流速和柱温对喹禾灵对映体分离效果的影响。结果表明,在正己烷-异丙醇(95∶5,体积比)为流动相,流速1.0 mL/min,柱温25℃的条件下,喹禾灵对映体能获得基线分离,分离度Rs为3.97,R-构型先出峰,两对映体的检出限均为0.045 mg/L,定量下限均为0.15 mg/L。在15～35℃柱温范围内,lnα对1/T Van't Hoff曲线呈良好的线性关系,相关系数(r2)大于0.99,分离因子α随温度升高而降低,焓变差和熵变差热力学参数显示,喹禾灵对映体的拆分过程受焓控制。The enantiomeric resolution of quizalofop-ethyl on Chiralpak IC column（cellulose-tris（3,5-dichlorophenylcarbamate） immonilized on silica） was studied.Effects of mobile phase composition,flow rate and temperature on the chiral separation of enantiomers were investigated.The result showed that a good baseline separation of quizalofop-ethyl enantiomers was obtained by using n-hexane-isopropanol（95∶5） as mobile phase with a flow rate of 1.0 mL/min at 25 ℃.The resolution was up to 3.97,in which R-enantiomer was firstly eluted.The limits of detection（LOD） for both of enantiomers were 0.045 mg/L and the limits of quantitation（LOQ） were 0.15 mg/L.The Van′t Hoff plot of the lnα versus 1/T showed a good linearity with correlation coefficients higher than 0.99 at column temperature of 15-35 ℃.The resolution factor was decreased with the increase of column temperature.The enthalpy and entropy change difference showed that the enantioseparation of quizalofop-ethyl enantiomers was enthalpy driven.

关 键 词：喹禾灵 手性拆分 Chiralpak IC柱 高效液相色谱 

分 类 号：O657.72[理学—分析化学] TQ457[理学—化学]