| 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 |
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| 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. |
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| 作者姓名： | 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 |
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| 作者单位： | 1.山东农业大学 植物保护学院, 山东 泰安 271018 |
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| 基金项目： | 山东省大型科学仪器设备升级改造技术研究专项(2013SJGZ06). |
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| 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。
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| 关 键 词： | 超高效液相色谱-串联质谱 硝磺草酮 代谢物 土壤 残留 |
| 收稿时间： | 2015/11/19 0:00:00 |
| 修稿时间： | 2016/3/28 0:00:00 |
Determination of mesotrione and its metabolite residues in soils by ultra performance liquid chromatography-tandem mass spectrometry |
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| DENG Ligang,CHEN Yebing,LI Zengmei,ZHAO Shancang,WANG Wenzheng,GUO Changying,WANG Lei,QIN Hongwei and 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. |
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| Authors: | DENG Ligang CHEN Yebing LI Zengmei ZHAO Shancang WANG Wenzheng GUO Changying WANG Lei QIN Hongwei and LU Fusui |
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| Institution: | 1.College of Plant Protection, Shandong Agricultural University, Tai'an 271018, Shandong Province, China2.Institute of Agricultural Quality Standards and Testing Technology Research, Shandong Academy of Agricultural Sciences/Key Laboratory of Test Technology on Food Quality and Safety of Shandong Province, Ji'nan 250100, China3.College of Chemistry and Materials Science, Shandong Agricultural University, Tai'an 271018, Shandong Province, China |
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| 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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| Keywords: | ultra performance liquid chromatography-tandem mass spectrometry mesotrione metabolites soil residue |
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