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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4.0 d,土壤中降解产物AMBA残留量高于MNBA。
A method for the determination of mesotrione and its metabolites 4-methylsulfone-2-nitrobenzoic acid (MNBA) and 2-amino-4-methylsulfonylbenzoic acid (AMBA) Tandem mass spectrometry (UPLC-MS / MS) analysis method. The samples were extracted with 0.1% aqueous ammonia-acetonitrile solution and purified on a Cleanert PAX SPE column. The mobile phase was acetonitrile and 0.3% formic acid. The mobile phase was eluted with an Acquity HSS T3 column. The electrospray anion-anion multiple reaction monitoring system UPLC- / MS test. The results showed that the average recoveries of mesotrione, MNBA and AMBA ranged from 73% to 97% and the relative standard deviations (RSDs) ranged from 2.4% to 12.9% at the level of 0.3-50 μg / kg. The detection limits were 0.1, 0.3 and 0.2 μg / kg, respectively. The limits of quantification were 0.3, 1.0 and 0.6 μg / kg, respectively. This method was applied to the laboratory simulation of laterite samples. The results showed that the half-life of mesotrione in soils was 4.0 days, and that of AMBA in soil was higher than MNBA.