邓立刚, 陈业兵, 李增梅, 赵善仓, 王文正, 郭长英, 王磊, 秦宏伟, 路福绥. 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[J]. 农药学学报, 2016, 18(3): 344-351. DOI: 10.16801/j.issn.1008-7303.2016.0047
    引用本文: 邓立刚, 陈业兵, 李增梅, 赵善仓, 王文正, 郭长英, 王磊, 秦宏伟, 路福绥. 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[J]. 农药学学报, 2016, 18(3): 344-351. DOI: 10.16801/j.issn.1008-7303.2016.0047
    DENG Ligang, CHEN Yebing, LI Zengmei, ZHAO Shancang, WANG Wenzheng, GUO Changying, WANG Lei, QIN Hongwei, LU Fusui. Determination of mesotrione and its metabolite residues in soils by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2016, 18(3): 344-351. DOI: 10.16801/j.issn.1008-7303.2016.0047
    Citation: DENG Ligang, CHEN Yebing, LI Zengmei, ZHAO Shancang, WANG Wenzheng, GUO Changying, WANG Lei, QIN Hongwei, LU Fusui. Determination of mesotrione and its metabolite residues in soils by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2016, 18(3): 344-351. DOI: 10.16801/j.issn.1008-7303.2016.0047

    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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