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

中文关键词:  固体萃取  水生蔬菜  农药残留  高效液相色谱-串联质谱法

英文关键词:solid phase extraction  aquatic vegetables  pesticide residues  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      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0.5~20.0 μg/kg、灭草松在0.5~10.0 μg/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0.030~0.170 μg/kg, 定量限为0.100~0.500 μg/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。

英文摘要:

      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 20.0 μg/kg, while bentazone showed linearity within the range of 0.5 to 10.0 μg/kg, with correlation coefficients reaching 0.99. The limits of detection ranged from 0.030 to 0.170 μg/kg, and the limits of quantitation were between 0.100 and 0.500 μg/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.