超高效液相色谱-串联质谱法测定土壤中硝磺草酮及其代谢物残留

    Determination of mesotrione and its metabolite residues in soils by ultra performance liquid chromatography-tandem mass spectrometry

    • 摘要: 建立了土壤中硝磺草酮及其代谢物4-甲砜基-2-硝基苯甲酸(MNBA)和2-氨基-4-甲砜基苯甲酸(AMBA)残留的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品用0.1%氨水-乙腈溶液提取后,经Cleanert PAX固相萃取柱净化,以乙腈和0.3%甲酸水为流动相,Acquity HSS T3色谱柱梯度洗脱,电喷雾负离子多反应监测模式UPLC-MS/MS检测。结果表明:在0.3~50μg/kg添加水平下,硝磺草酮、MNBA和AMBA的平均添加回收率在73%~97%之间,相对标准偏差在2.4%~12.9%之间,该方法的检出限分别为0.1、0.3和0.2μg/kg,定量限分别为0.3、1.0和0.6μg/kg。应用该方法对室内模拟试验的红土样品进行了分析,结果表明,硝磺草酮在红土中的消解半衰期为4.0d,土壤中降解产物AMBA残留量高于MNBA。

       

      Abstract: A comprehensive analytical method has been developed for the simultaneous determination of mesotrione and its metabolites (4-methylsulfonyl-2-nitrobenzoic acid (MNBA), 2-amino-4- (methylsulfonyl) benzoic acid (AMBA)) in soils by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-ESI-MS/MS). The soil samples were extracted with 0.1% ammonium hydroxide solution/acetonitrile and an aliquot of the extract was cleaned-up by a solid-phase extraction Cleanert PAX cartridge. The chromatographic separation was performed on an Acquity HSS T3 column with gradient elution using acetonitrile and 0.3% formic acid in water. The analytes were measured by multiple reaction monitoring (MRM) in the electrospray negative ionization mode. The recoveries were 73%-97% with the relative standard deviation from 2.4% to 12.9% for spiked soil samples at 0.3 μg/kg- 50 μg/kg. The limits of detection of mesotrione, MNBA and AMBA in soils were 0.1, 0.3 and 0.2 μg/kg, and the limits of quantifications of mesotrione, MNBA and AMBA were 0.3, 1.0 and 0.6 μg/kg. The analytical method has been employed in the simulation experiments with the red soil samples. The result showed that the half-life of mesotrione was 4.0 days in the red soil and the residue amounts of AMBA were higher than MNBA.

       

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