分散固相萃取超高效液相色谱串联质谱法同时检测大豆植株及土壤中烟嘧磺隆、莠去津及其代谢物残留

Simultaneous determination of nicosulfuron,atrazine,and their metabolites in soybean plants and soil by dispersive solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry

土壤中烟嘧磺隆和莠去津的高残留往往会导致后茬大豆药害问题。本研究建立了一种分散固相萃取超高效液相色谱串联质谱法同时检测大豆植株及土壤中烟嘧磺隆、莠去津及其代谢物残留方法。样品经含2%甲酸的乙腈提取,经分散固相萃取净化,以乙腈和0.2%甲酸水为流动相,采用Poroshell 120 EC-C18色谱柱梯度洗脱,基质匹配标准曲线外标法定量分析。结果表明:在0.01、0.10 mg/kg和1.00 mg/kg添加水平下,烟嘧磺隆、莠去津及其代谢物的平均回收率为70%~113%,相对标准偏差为0.3%~11.8%,目标化合物质量浓度与对应的峰面积之间在0.001~1 mg/kg范围内线性关系良好,决定系数R^(2)≥0.9841,方法的定量限为0.01 mg/kg。该方法简便、快捷、准确,适用于土壤和幼苗期至鼓粒期大豆植株中烟嘧磺隆、莠去津及其代谢物的检测。本研究为烟嘧磺隆和莠去津的科学使用及后茬作物的安全种植提供有效监测方法。

High nicosulfuron and atrazine residues in the soil often lead to the phytotoxicity of subsequent soybeans.In this study,a method was established for simultaneous determination of nicosulfuron,atrazine,and their metabolites in soybean plants and soil by dispersive solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry.The samples were extracted with acetonitrile(containing 2%formic acid)and purified by dispersive solid-phase extraction.The separation of target compound was achieved on an Poroshell 120 EC-C18 chromatographic column using acetonitrile and 0.2%formic acid water as mobile phases.The purified samples were then quantitatively analyzed by the external standard method using matrix-matched calibration curves.The results showed that the mean recoveries of nicosulfuron,atrazine,and their metabolites ranged from 70%to 113%and the relative standard deviations ranged from 0.3%to 11.8%at three spiked levels of 0.01,0.10,and 1.00 mg/kg.The linear relationships between the mass concentration of the target compound and the corresponding peak area were good in the range of 0.001-1 mg/kg with the correlation coefficients all higher than 0.9841.The limits of quantification(LOQs)of the method were 0.01 mg/kg.The developed method is convenient,rapid,and accurate,which can be applied for the simultaneous detection of nicosulfuron,atrazine,and their metabolites in soil and soybean plants from seedling stage to seed-filling stage.This study provides an effective monitoring method for the scientific use of nicosulfuron and atrazine and the safe planting of subsequent crops.