固相萃取/高效液相色谱-串联质谱法测定烟叶中春雷霉素残留量  

Determination of Kasugamycin Residues in Fresh and Cured Tobacco Leaves by Solid Phase Extraction/High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：张贵群[1,2,3] 郭素静 梁贵平 梁骥[1,2,3] 刘义珂 曾利红[1,2] 侯根连 ZHANG Gui-qun;GUO Su-jing;LIANG Gui-ping;LIANG Ji;LIU Yi-ke;ZENG Li-hong;HOU Gen-lian(National Engineering Research Center for Agrochemicals,Hunan Research Institute of Chemical Industry Changsha 410014,China;Hunan Province Key Laboratory for Agrochemicals,Changsha 410014,China;Hunan J&F Test Co.,Ltd.,Changsha,410014,China;Institute for the Control of Agrochemicals,Ministry of Agriculture and Rural Affairs,Beijing 100125,China)

机构地区：[1]湖南化工研究院国家农药创制工程技术研究中心,湖南长沙410014 [2]农用化学品湖南省重点实验室,湖南长沙410014 [3]湖南加法检测有限公司,湖南长沙410014 [4]农业农村部农药检定所,北京朝阳100125

出　　处：《精细化工中间体》2020年第3期73-76,共4页Fine Chemical Intermediates

基　　金：国家药典委员会药品审评审批制度综合改革项目(ZG-2016-08)。

摘　　要：建立了固相萃取/高效液相色谱-串联质谱(SPE/HPLC-MS/MS)测定烟叶中春雷霉素残留量的分析方法。样品经0.1%甲酸的甲醇水溶液(7∶3,v/v)超声提取后,采用混合型阳离子(PCX)小柱净化,以Kinetex PFP色谱柱分离,采用UPLC-MS/MS多反应监测(MRM)正离子模式测定,外标法定量。春雷霉素在烟叶中的最低检测浓度为0.05 mg·kg^-1,在0.05、0.50、2.00 mg·kg^-13个添加水平下,平均回收率为78%~87%,相对标准偏差为3%~8%。A method of determination for kasugamycin in tobacco leaves by HPLC-MS/MS was established.The analytes were extracted from samples using 0.1%formic acid methanol and water solution(7+3,v/v),and purified with PCX solid phase extraction columns,then analyzed using UPLC-MS/MS multiple reaction monitoring(MRM)mode via positive electrospray ionization with a Waters Kinetex PFP column as the analytical column.All the analytes were quantified by the external standard method.The limit of quantification was 0.05 mg·kg^-1.The results showed that the average recoveries at the fortified levels of 0.05,0.50,2.00 mg·kg^-1 ranged from 78%to 87%,and the RSD were 3%~8%.

关 键 词：高效液相色谱-串联质谱 春雷霉素 残留 烟叶 

分 类 号：O657.7[理学—分析化学]