固相萃取-高效液相色谱-串联质谱法同时测定水生蔬菜中的5种农药残留  

Simultaneous determination of 5 kinds of pesticide residues in aquatic vegetables by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

作　　者：许嘉[1] 王硕[1] 王银会[1] 孙佳林 XU Jia;WANG Shuo;WANG Yin-Hui;SUN Jia-Lin(Beijing Chaoyang Center for Disease Control and Prevention,Beijing 100021,China)

机构地区：[1]北京市朝阳区疾病预防控制中心,北京100021

出　　处：《食品安全质量检测学报》2024年第23期174-181,共8页Journal of Food Safety and Quality

基　　金：2022年冬奥会突发公共卫生事件应急保障技术平台建设项目(CYSF2011)。

摘　　要：目的建立固体萃取-高效液相色谱-串联质谱法测定水生蔬菜中甲基对硫磷、灭草松、莠去津、呋喃丹和2,4-滴的分析方法。方法待测样品均质后加入0.2%甲酸乙腈、氯化钠溶液超声提取30 min,经C18固相萃柱净化后,使用Waters UPLC HSS T3色谱柱进行分离,流动相为0.1%甲酸水溶液-甲醇溶液,以电喷雾离子源采用多离子反应监测模式检测。结果甲基对硫磷、莠去津、呋喃丹和2,4-滴在0.5~20.0μg/kg、灭草松在0.5~10.0μg/kg的浓度范围内具有良好的线性关系,相关系数达到了0.99。检出限为0.030~0.170μg/kg,定量限为0.100~0.500μg/kg。6个不同加标水平的平均加标回收率为86.4%~110.3%,相对标准偏差为0.87%~8.34%。结论本研究建立的方法简便,准确度高,精密度好,重现性强,适用于同时测定水生蔬菜中甲基对硫磷、灭草松、莠去津、呋喃丹和2,4-滴的5种农药残留量。Objective To establish a method for the determination of methyl parathion,bentazone,atrazine,carbofuran,and 2,4-D in aquatic vegetables by solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry.Methods After homogenizing the test samples,0.2%formic acid in acetonitrile and sodium chloride solution were added,followed by ultrasonic extraction for 30 minutes.After purification using a C18 solid phase extraction column,the samples were separated using a Waters UPLC HSS T3 chromatographic column with a mobile phase consisting of 0.1%formic acid in water and methanol.Detection was performed using an electrospray ionization source in multiple reaction monitoring mode.Results Methyl parathion,atrazine,carbofuran,and 2,4-D exhibited good linearity within the concentration range of 0.5 to 20.0μg/kg,while bentazone showed linearity within the range of 0.5 to 10.0μg/kg,with correlation coefficients reaching 0.99.The limits of detection ranged from 0.030 to 0.170μg/kg,and the limits of quantitation were between 0.100 and 0.500μg/kg.The average spiked recovery rates at 6 kinds of different spiking levels were between 86.4%and 110.1%,with relative standard deviations ranging from 0.87%to 8.34%.Conclusion The method established in this study is simple,highly accurate,precise,and reproducible,making it suitable for the simultaneous determination of 5 kinds of pesticide residues,namely methyl parathion,bentazone,atrazine,carbofuran,and 2,4-D in aquatic vegetables.

关 键 词：固体萃取 水生蔬菜 农药残留 高效液相色谱-串联质谱法 

分 类 号：TS254.58[轻工技术与工程—水产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]