高效液相色谱-串联质谱法同步检测大麦产品中唑啉草酯、炔草酯及解毒喹的残留量  

Simultaneous Determination of Pinoxaden and Clodinafop-Propargyl and Cloquintocet-Mexyl Residues in Barley by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：韩何丹 佘永新[3] 贺永娟 何亚荟 王猛强 王淼[3] 王珊珊[3] 郑鹭飞[3] 曹振 邵华[3] 金茂俊[3] 金芬[3] 王静[3] 高丽萍[1,2] HAN Hedan;SHE Yongxin;HE Yongjuan;HE Yahui;WANG Mengqiang;WANG Miao;WANG Shanshan;ZHENG Lufei;CAO Zhen;SHAO Hua;JIN Maojun;JIN Fen;WANG Jing;GAO Liping(College of Biochemical Engineering,Beijing Union University,Beijing 100023,China;Beijing Municipal Key Laboratory of Biologically Active Substances and Functional Food,Beijing 100191,China;Institute of Quality Standard and Testing Technology for Agro-products,Chinese Academy of Agricultural Sciences,Beijing 100081,China)

机构地区：[1]北京联合大学生物化学工程学院,北京100023 [2]生物活性物质与功能食品北京市重点实验室,北京100191 [3]中国农业科学院农业质量标准与检测技术研究所,北京100081

出　　处：《食品科学》2020年第6期292-297,共6页Food Science

基　　金：现代农业产业技术体系建设专项(CARS-05-05A-03);国家自然科学基金面上项目(31471654;31772071)。

摘　　要：利用QuEChERS提取建立高效液相色谱-串联质谱法同时检测大麦中的除草剂唑啉草酯和炔草酯及解毒喹的残留。样品用乙腈提取,C18和N-丙基乙二胺净化,在XBridge-C18色谱柱上分离,以0.1%甲酸溶液和乙腈作为流动相进行梯度洗脱,电喷雾电离正离子模式扫描,多反应监测测定,基质匹配外标法定量分析。大麦粒中唑啉草酯、炔草酯和解毒喹在0.1~100μg/L范围内呈线性关系,相关系数不低于0.9996;方法的检出限分别为0.05、0.02μg/L和0.01μg/L。唑啉草酯、炔草酯和解毒喹的精密度实验中3个加标水平(以国家标准中小麦对其残留限量为参考)平均回收率在76.87%~103.55%之间,相对标准偏差在2.4%~9.2%(n=5)之间。采用该方法对当地市场的大麦麦粒和大麦苗粉中3种化合物的残留进行应用性评价,该方法将为大麦产品中唑啉草酯等3种化合物的残留检测提供一定技术支撑。An analytical method for simultaneous determination of the results of two herbicides,pinoxaden,clodinafoppropargyl,and the herbicide safety agent cloquintocet-mexyl in barely was developed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)combined with quick,easy,cheap,effective,rugged,and safe(QuEChERS)extraction.The samples were extracted with acetonitrile,and cleaned up with C18 and N-propyl ethylenediamine(PSA).The analytes were then separated with a reversed phase C18 column(XBridge)by gradient elution with a mixture of 0.1%formic acid solution and acetonitrile as the mobile phase.The instrument was operated under the multiple reaction monitoring(MRM)mode with positive electrospray ionization and the analytes were quantified by matrix matched external standard method.Good linearity was obtained in the concentration range of 0.1–100μg/L with correlation coefficients no less than 0.9996.The limits of detection(LODs)of the method were 0.05,0.02 and 0.01μg/L for pinoxaden,clodinafop-propargyl and cloquintocet-mexyl,respectively.The average recoveries of the analytes at three spiked concentration levels(determined according to the residue limits of the national standard for wheat)were 76.87%–103.55%.The repeatability,expressed as relative standard deviations(RSD),ranged from 2.4%to 9.2%(n=5).The method confirmed its applicability to marketed barley grains and seedling flour.This method provides technical support for the determination of pinoxaden residues in barley products.

关 键 词：大麦 唑啉草酯 炔草酯 解毒喹 QuEChERS 高效液相色谱-串联质谱 

分 类 号：S482.4[农业科学—农药学] O657.72[农业科学—植物保护]