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首页> 外文期刊>Chromatographia >Determination of Chlorantraniliprole Residues in Corn and Soil by UPLC–ESI–MS/MS and Its Application to a Pharmacokinetic Study
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Determination of Chlorantraniliprole Residues in Corn and Soil by UPLC–ESI–MS/MS and Its Application to a Pharmacokinetic Study

机译:UPLC-ESI-MS / MS法测定玉米和土壤中的氯氰菊酯残留量及其在药代动力学研究中的应用

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A rapid, highly sensitive, and selective method was developed for the determination of the insecticide chlorantraniliprole (CAP) in corn and soil using ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS). Samples were extracted with acetonitrile, and aliquots were cleaned with solid-phase extraction cartridges. Two precursor-product ion transitions for CAP were measured and evaluated to provide maximum confidence in the results. Average recovery for soil, corn grain, and corn straw at different levels (5 or 10, 40, and 100 μg kg−1) ranged from 74.9 to 97.5%, with intra-day relative standard deviation (RSD) values of 1.9–11.3% and inter-day RSD values of 4.7–10.4%. Coefficients of determination (R 2) of 0.9988 or higher were achieved for CAP in soil, corn grain, and corn straw matrix calibration curves, from 5 to 1,000 μg L−1. The CAP limits of quantitation in soil, corn grain, and straw were determined to be 5, 10, and 10 μg kg−1, respectively, which were much lower than the maximum residue levels established by the Environmental Protection Agency of United States. UPLC–MS/MS was used to determine the CAP residues in real corn and soil for studies on their dissipation. The trial results showed that the half-lives of CAP changed from 12.6 to 23.1 days in soils and ranged from 4.9 to 5.4 days in corn straws in the districts of Henan and Shandong, and the average levels of CAP residues in corn grains were all <0.01 mg kg−1 with a harvest withholding period of 180 days.
机译:建立了一种快速,高度灵敏和选择性的方法,采用超高效液相色谱-串联质谱法(UPLC-MS / MS)测定玉米和土壤中的杀虫剂绿蒽酮(CAP)。样品用乙腈萃取,等分试样用固相萃取柱清洁。测量并评估了CAP的两个前体产物离子跃迁,以提供最大的置信度。不同水平(5或10、40和100μgkg -1 )下的土壤,玉米粒和玉米秸秆的平均回收率在74.9%至97.5%之间,且具有日内相对标准偏差( RSD)值为1.9-11.3%,日间RSD值为4.7-10.4%。在土壤,玉米粒和玉米秸秆基质校准曲线中,CAP的测定系数(R 2 )达到0.9988或更高,L −1 为5至1,000μg 。确定土壤,玉米粒和稻草中的CAP限量分别为5、10和10μgkg -1 ,这远低于环境署规定的最大残留量美国保护局。 UPLC-MS / MS用于确定真实玉米和土壤中的CAP残留量,以研究它们的耗散情况。试验结果表明,在河南和山东地区,土壤中CAP的半衰期从12.6改变为23.1天,在玉米秸秆中的半衰期从4.9改变为5.4天,玉米籽粒中的CAP残留平均水平均< 0.01 mg kg -1 ,保留期为180天。

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