高效液相色谱-串联质谱法结合多糖衍生物手性固定相拆分氰戊菊酯  

Resolution of fenvalerate by high performance liquid chromatography-tandem mass spectrometry coupled with chiral stationary phase of polysaccharide derivatives

作　　者：董超 李晶 杨秦 安文进 张耀海 赵其阳[1,2,3] 焦必宁 DONG Chao;LI Jing;YANG Qin;AN Wenjin;ZHANG Yaohai;ZHAO Qiyang;JIAO Bining(Quality and Safety Risk Assessment Laboratory for Citrus Products in the Ministry of Agriculture and Rural Areas(Chongqing),Chongqing 400712;Citrus and Seedling Quality Supervision and Testing Center,Ministry of Agriculture and Rural Sciences,Chongqing 400712;Institute of Citrus,Southwest Agricultural University,Chongqing 400712)

机构地区：[1]农业农村部柑桔产品质量安全风险评估实验室(重庆),重庆400712 [2]农业农村部柑桔及苗木质量监督检验测试中心,重庆400712 [3]中国农业科学院/西南大学柑桔研究所,重庆400712

出　　处：《分析试验室》2020年第4期448-453,共6页Chinese Journal of Analysis Laboratory

基　　金：农业农村部现代农业(柑橘)产业技术体系建设专项(CARS-26);国家柑橘及热带作物产品质量安全风险评估专项(GJFP2018004)资助。

摘　　要：建立了以多糖衍生物为手性固定相的高效液相色谱-串联质谱(HPLC-MS/MS)直接拆分氰戊菊酯对映体的方法。在反相液相色谱条件下,考察了手性固定相的种类、流动相组成、柱温、流速对氰戊菊酯4个立体异构体分离的影响。同时,利用热力学方法对氰戊菊酯的立体异构体与固定相之间的色谱保留和分离的热力学机理进行了探讨。结果表明:采用Lux Cellulose-3(纤维素-三(4-甲基苯甲酸酯))手性色谱柱,在以流动相为乙腈-水(5 mmol/L甲酸铵)=(55:45,V:V)流速0.4 mL/min,柱温30℃的条件下,可在14 mins内实现氰戊菊酯4个立体异构体的基线分离。拓展了HPLC-MS/MS在菊酯类手性农药对映体分离及检测上的应用。A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method based on polysaccharide-based chiral stationary phases(CSPs)was established to separate fenvalerate.The effects of chiral immobilization,mobile phase composition,column temperature and flow rate on the separation of 4 stereoisomers of fenvalerate were investigated under reversed-phase liquid chromatographic conditions.Meanwhile,the thermodynamic mechanism of chromatographic retention and separation between the stereoisomers of fenvalerate and the stationary phase was discussed using thermodynamic methodology.The results showed that the baseline separation of the 4 stereoisomers of fenvalerate could be achieved via a Lux Cellulose-3 chiral column using the mobile phase of acetonitrile-water(5 mmol/L ammonium formate)at a flow rate of 0.4 mL/min and a column temperature of 30°C within 14 minutes.The present investigation expands the application of HPLC-MS/MS in the separation and determination of chiral pyrethroid pesticides.

关 键 词：手性分离 氰戊菊酯 多糖衍生物手性固定相 分离 

分 类 号：O656.2[理学—分析化学]