分散固相萃取-超高效液相色谱-串联质谱法同时检测玉米及其土壤中烟嘧磺隆、莠去津及氯氟吡氧乙酸残留  

Simultaneous determination of nicosulfuron,atrazine and fluroxypyr in soil and corn by ultraperformance liquid chromatography-mass spectrometry

作　　者：郭立群[1,2] 徐军[2] 董丰收[2] 刘新刚[2] 郑永权[2] 

机构地区：[1]东北农业大学农学院,哈尔滨150030 [2]中国农业科学院植物保护研究所/农业部农药化学与应用重点开放实验室,北京100193

出　　处：《农药学学报》2012年第2期177-184,共8页Chinese Journal of Pesticide Science

基　　金：国家自然科学基金项目(31000863)

摘　　要：采用QuEChERS法结合超高效液相色谱-串联质谱法(UPLC-MS/MS)建立了玉米及其土壤中同时检测烟嘧磺隆、莠去津和氯氟吡氧乙酸残留的分析方法。样品采用乙腈(含体积分数为2%的甲酸)提取,基质固相分散净化后,用UPLC-MS/MS外标法检测定量。结果表明:该方法具有灵敏度高、简便、快速等优点;在0.01～1.0 mg/L质量浓度范围内,3种除草剂的仪器响应值与其质量浓度呈良好线性相关,相关系数大于0.990 6;玉米和土壤样品中3种除草剂的添加水平在0.02～0.5 mg/kg时,平均回收率均为78.9%～117.7%,日内相对标准偏差(RSD)均小于11.6%,日间RSD均小于13.9%。3种除草剂在玉米籽粒、玉米植株和土壤中的定量限(LOQ)均小于7.1μg/kg。A rapid analytical method for simultaneous determination of nicosulfuron,atrazine and fluroxypyr in corn and soil was established based on QuEChERS with ultraperformance liquid chromatography-mass spectrometry（UPLC-MS/MS）.Residues were firstly extracted with acetonitrile（containing 2% formic acid）,and then detected by UPLC-MS/MS with external standard method after being cleaned up with matrix solid-phase dispersion.The results showed that the established method was rapid,simple,high efficient and sensitive.A good linearity ranged from 0.01-1.0 mg/L was obtained and correlation coefficient was higher than 0.990 6.The average recoveries of the three herbicides in different matrices were in the range of 78.9%-117.7% at spiked levels 0.02-0.5 mg/kg,with intra-day relative standard deviations lower than 11.6% and inter-day relative standard deviations lower than 13.9%.The limits of quantification（LOQ） of three pesticides in corn and soil were lower than 7.1 μg/kg.

关 键 词：超高效液相色谱-串联质谱 QuEChERS 玉米 土壤 农药残留 

分 类 号：O657.63[理学—分析化学]