玉米中9种磺酰脲类除草剂的超高效液相色谱-串联质谱法同时测定  

Simultaneous Determination of 9 Sulfonylurea Herbicides in Corn Using Solid-phase Extraction and Ultra Performance Liquid Chromatography with Electrospray Ionization Tandem Mass Spectrometry

作　　者：丁菲[1,2] 李范珠[1] 储晓刚[2] 张峰[2] 凌云[2] 孙利[2] 杨敏莉[2] 吕泉福[2,3] 许成保 

机构地区：[1]浙江中医药大学药学院,浙江杭州310053 [2]中国检验检疫科学研究院,北京100123 [3]西南大学药学院,重庆400715

出　　处：《分析测试学报》2011年第1期53-57,共5页Journal of Instrumental Analysis

基　　金：质检公益性行业科研项目(200910145);国家科技支撑计划资助项目(2009BADB9B02);国家质检总局科技计划资助项目(2008IK167);北京市科技计划资助项目(D08050200310803)

摘　　要：采用超高效液相色谱-串联四极杆质谱（UPLC～MS／MS），在多反应监测（MRM）模式下建立了玉米中9种磺酰脲类除草剂残留的定性定量分析方法。样品浸泡后采用甲醇-丙酮（体积比1：1）提取、浓缩，经C18固相萃取柱净化处理。采用UPLC—ESIMS／MS方法测定，外标法定量。9种磺酰脲类除草剂在0．05～2．0mg·L^-1范围内具有较好的线性关系，相关系数均大于0．99，该方法的检出限（LOD，S／N=3）为0．001～0．005mg·L^-1，定量下限（LOQ，S／N=10）为0．062～0．080mg·kg^-1。在1LOQ、2LOQ和5LOQ3个加标水平下的回收率为60％～85％，相对标准偏差（RSDs）均在10％以内。该方法简便快速，满足玉米中9种磺酰脲类除草剂的快速检测要求。A new method based on solid phase extraction and ultra performance liquid chromatography- tandem mass spectrometry（ UPLC -ESI MS/MS） was developed for the determination of 9 sulfonylurea herbicides（metoxuron, foramsulfuron, cinosulfuron, methabenthiazuron, prosulfuron, linuton, ethoxysulfuron, chloroxuron and cyclosulfamuron） in corn. The corn sample was soared in water, and then extracted with methanol - acetone （ 1 ： 1, by volume）. The extract was cleaned up by C18 solid phase extraction cartridge. The eluent was evaporated to near dryness under a stream of nitrogen gas, and redissolved by methanol. The identification and detection of target compounds were achieved under multiple reactions monitoring （MRM） mode with positive electrospray ionization （ESI）. 9 sulfonylurea herbcides were quantified by external standard method. The calibration curves of 9 sulfonylurea herbicides were linear in the range of 0.05 - 2.0 mg·L^-1 with correlation coefficients more than 0. 99. The limits of detection （ LOD, S/N = 3 ） and the limits of quantitation （ LOQ, S/N = 10） were in the range of 0.001 - 0. 005 mg - L ^-1 and 0. 062 - 0. 080 mg· kg^-1, respectively, 1 LOQ, 2LOQ and 5LOQ were chosen as the three spiked levels of recovery for the method. The recoveries of 9 sulfonylurea herbicides ranged from 60% to 85% with relative standard deviations less than 10% . The method was simple and effective, and could meet the requirements the simultaneous determination of 9 sulfonylurea herbicides in corn sample.

关 键 词：固相萃取 超高效液相色谱-电喷雾串联质谱 磺酰脲类除草剂 玉米 

分 类 号：O657.63[理学—分析化学] S482.4[理学—化学]