液相色谱-串联质谱法测定植物源性食品中总氟吡禾灵残留  

Determination of Total Haloxyfop in Plant-derived Foods by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王兴宁 王涛[2] 李洁 李志 唐亚峰 梁艺馨 朱明 WANG Xing-ning;WANG Tao;LI Jie;LI Zhi;TANG Ya-feng;LIANG Yi-xin;ZHU Ming(Center for Comprehensive Technology of Guiyang Customs,Guiyang 550081,China;Guizhou Light Industrial Vocational College,Guiyang 540003,China)

机构地区：[1]贵阳海关综合技术中心,贵州贵阳550081 [2]贵州轻工职业技术学院,贵州贵阳540003

出　　处：《分析测试学报》2021年第10期1526-1531,共6页Journal of Instrumental Analysis

基　　金：国家重点研发计划(2017YFC1601603);海关总署科研项目(2019HK122)。

摘　　要：应用液相色谱-串联质谱(LC-MS/MS)技术,建立了植物源性食品中总氟吡禾灵的测定方法。样品经碱性乙腈提取,用无水MgSO_(4)、十八烷基硅烷(C_(18))和石墨化炭黑(GCB)基质分散固相萃取净化。采用0.1%甲酸乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,C_(18)色谱柱(2.1 mm×50 mm,1.7μm)分离,在正离子模式下采用多反应监测(MRM)扫描测定,内标法定量。结果表明:氟吡禾灵在2.5~50 ng/mL范围内线性关系良好,相关系数(r^(2))大于0.999;0.01、0.05、0.1 mg/kg 3个加标水平下,柠檬、柑橘、马铃薯、结球甘蓝、甜椒、洋葱、大米、葵花籽及茶叶9种基质的平均回收率为80.7%~114%,相对标准偏差(RSD)为1.4%~11%;方法定量下限为0.01 mg/kg。该方法显示氟吡禾灵酯类完全转化为总氟吡禾灵,适用于植物源性食品中总氟吡禾灵的快速检测。A simple,fast and reliable method was developed for quantitative determination of total haloxyfop in plant-derived foods using liquid chromatography coupled to tandem mass spectrometry(LC-MS/MS).The sample preparation consisted of a dispersive solid phase extraction(dispersive-SPE)method by addition of an alkaline hydrolysis step to release total haloxyfop.The target com⁃pound was extracted with acetonitrile,and then purified using anhydrous MgSO_(4),octadecyl(C_(18))and graphitized carbon black(GCB).A mixture of 0.1%formic acid acetonitrile and 0.1%formic acid aqueous solution was used as the mobile phase,followed by binary gradient elution,C_(18)(2.1 mm×50 mm,1.7μm)column separation.The analysis was performed in positive ion mode under mul⁃tiple reaction monitoring(MRM)mode,and internal standard method was used for quantitative analy⁃sis.Results showed that there was a good linear relationship for haloxyfop over the range of 2.5-50 ng/mL with a correlation coefficient(r^(2))greater than 0.999.At three spiked levels(0.01,0.05 and 0.1 mg/kg),average recoveries for total haloxyfop ranged from 80.7%to 114%,with relative standard deviations(RSD)of 1.4%-11%.The limit of quantitation was as low as 0.01 mg/kg.The method showed a fully converted step from haloxyfop-esters to haloxyfop,and it was suitable for the analysis of total haloxyfop residues in plant-derived foods.

关 键 词：总氟吡禾灵 碱水解 分散固相萃取 植物源性食品 液相色谱-串联质谱 

分 类 号：O657.7[理学—分析化学] TS201.6[理学—化学]