分析测试学报2011，Vol.30Issue(1)：53-57,5.DOI:10.3969/j.issn.1004-4957.2011.01.011
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
摘要
Abstract
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, linuron, 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 nitregen 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 O. 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. 1LOQ,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Key words
SPE/ ultra performance liquid chromatography - tandem mass spectrometry/ sulfonylurea herbicides/ corn分类
化学化工引用本文复制引用
丁菲,李范珠,储晓刚,张峰,凌云,孙利,杨敏莉,吕泉福,许成保..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[J].分析测试学报,2011,30(1):53-57,5.基金项目
质检公益性行业科研项目(200910145) （200910145）
国家科技支撑计划资助项目(2009BADB9B02) （2009BADB9B02）
国家质检总局科技计划资助项目(2008IK167) （2008IK167）
北京市科技计划资助项目(D08050200310803) （D08050200310803）
