超高效液相色谱-串联质谱法测定油料作物中8种苯胺类除草剂  

Determination of 8 Aniline Herbicides in Oil Crops by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：郭爱静[1] 花中霞[1] 辛佳 张弘[1] 张世勇[1] 曹丽玲[1] 王可[1] GUO Aijing;HUA Zhongxia;XIN Jia;ZHANG Hong;ZHANG Shiyong;CAO Liling;WANG Ke(Shijiazhuang Technology Innovation Center for Chemical Poison Detection and Risk Early Warning,Shijiazhuang Center for Disease Control and Prevention,Shijiazhuang 050011,China)

机构地区：[1]石家庄市疾病预防控制中心,石家庄市化学毒物检测及风险预警技术创新中心,河北石家庄050011

出　　处：《食品工业科技》2021年第2期204-209,共6页Science and Technology of Food Industry

基　　金：石家庄市科学技术研究与发展指导计划(191460733);河北省医学适用技术跟踪项目(GZ2020042)。

摘　　要：建立了玉米、花生等油料作物中8种苯胺类除草剂的超高效液相色谱-串联质谱检测方法。试样经乙腈超声提取后,以N-丙基乙二胺(N-propyl ethylenediamine,PSA)和无水MgSO4净化,ZORBAX Eclipse Plus C(18)色谱柱(2.1 mm×100 mm,1.8μm)分离,以甲醇(含1%乙腈)和5 mmol/L乙酸铵水溶液(含0.1%甲酸)为流动相梯度洗脱,流速为0.3 mL/min。采用电喷雾离子源(ESI)正离子模式扫描,多反应监测(MRM)模式进行检测,外标法定量。结果表明,8种苯胺类除草剂在不同浓度范围内(二甲戊乐灵、仲丁灵和磺草唑胺在2.0~200μg/L,异丙乐灵在5.0~200μg/L,甲磺乐灵、乙酰甲草胺、氯苯胺灵和氯草灵在0.5~200μg/L)线性关系良好,相关系数(r)均在0.999以上,在3个不同浓度加标水平下的平均回收率为69.5%~97.5%,相对标准偏差(RSD,n=5)为0.5%~9.5%。方法的检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.07~1.20和0.23~4.00μg/kg。该方法高效、灵敏,适用于玉米和花生等油料作物中苯胺类除草剂的快速定量检测。A method was developed for the simultaneous determination of 8 aniline herbicides in oil crops by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were ultrasonically extracted with acetonitrile,and then purified with N-propyl ethylenediamine(PSA)and anhydrous magnesium sulfate.The target compounds were separated on a ZORBAX Eclipse Plus C 18 column(2.1 mm×100 mm,1.8μm)by gradient elution using methanol(containing 1%acetonitrile)and 5 mmol/L ammonium acetate solution(containing 0.1%formic acid)as mobile phase at a flow rate of 0.3 mL/min.Qualification was achieved by positive electro-spray ionization using multiple reaction monitoring(MRM),and the external standard method was used for quantitation.The calibration curves for 8 aniline herbicides were linear in their corresponding range(2.0~200μg/L for pendimethalin,butralin and metosulam,5.0~200μg/L for isopropalin,0.5~200μg/L for nitralin,diethatyl ethyl,chlorpropham and chlorbufam)with their correlation coefficients(r)all above 0.999.The recoveries for 8 aniline herbicides at three different spiked levels were in the range of 69.5%~97.5%with relative standard deviations(RSD)of 0.5%~9.5%(n=5).The limits of detection(S/N=3)and quantitation(S/N=10)of the method were 0.07~1.20 and 0.23~4.00μg/kg,respectively.Owing to high efficiency and sensitivity,the method was suitable for rapid and simultaneous analysis of aniline herbicides in oil crops.

关 键 词：超高效液相色谱-串联质谱(UPLC-MS/MS) 苯胺类除草剂 油料作物 

分 类 号：TS227[轻工技术与工程—粮食、油脂及植物蛋白工程]