QuEChERS结合HPLC-MS/MS法测定鲜烟叶中的2种抑芽剂  

Determination of Two Suckercides in Fresh Tobacco Leaves by Modified QuEChERS-HPLC-MS / MS

作　　者：艾小勇[1,2] 任志芹 袁飞[2] 李伟青[2] 张元[2] 原保忠[1] 张峰[2] 

机构地区：[1]华中农业大学植物科学技术学院,武汉430070 [2]中国检验检疫科学研究院烟草安全与控烟技术中心,北京100123 [3]河北农业大学理学院,河北保定071001

出　　处：《湖北农业科学》2016年第11期2888-2891,2920,共5页Hubei Agricultural Sciences

基　　金：国家重大仪器设备开发专项(2012YQ14000806);质检公益性行业科研专项(201310134);国家质检总局科技计划项目(2013IK202);质检公益科研性行业专项(201410088);茶叶及烟草中香精高通量筛查及精准鉴定方法专项(201410088-02)

摘　　要：建立鲜烟叶中二甲戊乐灵、仲丁灵2种抑芽剂的高效液相色谱-串联质谱（HPLC-MS/MS）检测方法。以乙腈为提取溶剂,对鲜烟叶中2种抑芽剂进行提取,采用新型复合吸附剂的Qu ECh ERS净化方法,用N-丙基乙二胺（PSA）、C18和石墨化碳黑（GCB）3种复合吸附剂净化,HPLC-MS/MS测定,以电喷雾正离子模式（ESI＋）,i Funnel离子聚焦,多反应监测（MRM）模式下进行检测,基质匹配外标法定量。通过优化条件,在10~500μg/kg范围内,二甲戊乐灵、仲丁灵的检测线性相关系数（R2）均大于0.995,检出限（LOD）为1.5~2.4μg/kg,定量限（LOQ）为5.0~7.9μg/kg,在3个添加水平下的回收率范围88.1%~96.4%,相对标准偏差（RSD）为3.2%~9.3%。试验方法可用于鲜烟叶中二甲戊乐灵、仲丁灵抑芽剂的准确测定。A HPLC-MS / MS method was established for the simultaneous determination of two suckercides of pendimethalin and butralin in fresh tobacco leaves. The two suckercides in fresh tobacco leaves were extracted by acetonitrile,purified by modified Qu ECh ERS purification method using new compound abrorbents of primary secondary amine（PSA）,graphitized carbon black（GCB） and C18,and then tested by HPLC-MS / MS under positive electrospray ionation（ESI＋）,i Funnel ionic focucing and multiple reaction monitoring（MRM） modes,with matrix matching and quantification of external standard method. Under the optimized conditions,two suckercides were observed good linear in the range of 10-500 μg / kg,with R2=0.995. The limits of detection（LOD） and the limits of quantification（LOQ） for two suckercides were 1.5-2.4 μg / kg and 5.0-7.9 μg / kg respectively.The average recoveries at three spiked concentration levels were within 88.1%~96.4%. The relative standard deviation（RSD）of these components ranged from 3.2% to 9.3%. The method could be used for the determination of pendimethalin and butralin residues in fresh tobacco leaves.

关 键 词：QUECHERS 复合吸附剂 抑芽剂 鲜烟叶 高效液相色谱-串联质谱(HPLC-MS/MS) 

分 类 号：O657.7[理学—分析化学] TS411[理学—化学]