分散固相萃取/超高效液相色谱-串联质谱法测定玉米和土壤中噻酮磺隆-异唑草酮及其代谢物残留

建立了分散固相萃取结合超高效液相色谱-串联质谱快速检测玉米和土壤中噻酮磺隆、异嚼唑草酮及其代谢物RPA203328与RPA202248残留的分析方法.样品经1％甲酸-乙腈溶剂提取,氯化钠盐析后,提取液经分散固相萃取净化,超高效液相色谱-串联质谱仪检测.考察了提取溶剂及吸附剂种类对分析结果的影响,优化了液相色谱-质谱条件,评估了优化实验条件下的方法性能.结果表明:在玉米样品中,4种分析物的基质效应均大于10％;在土壤样品中,除RPA202248基质效应小于10％外,其余3种分析物的基质效应均大于10％.噻酮磺隆、异唑草酮及其代谢物在0.001 ～ 1.0 μg/mL范围内线性关系良好,相关系数为0.994 5 ～0.999 5.加标浓度在0.005 ～0.1 mg/kg范围内的回收率为72.9％～ 116.5％,相对标准偏差(n=5)为0.75％ ～ 17.8％,定量下限为0.005 ～0.01 mg/kg.该方法前处理简单,分析时间短,准确度和灵敏度高,适用于玉米和土壤中噻酮磺隆、异唑草酮及其代谢物残留的快速检测.

Determination of Thiencarbazone-methyl,Isoxaflutole and their Metabolites Residues in Corn and Soil by Dispersive Solid-phase Extraction Combined with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A new method was established for the determination of thiencarbazone-methyl,isoxaflutole and their metabolites RPA203328 and RPA202248 residues in corn and soil by dispersive solid-phase extraction (d-SPE) combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with acidified acetonitrile(containing 1％ formic acid),and acetonitrile phase was separated from sample solution through salting-out phenomenon with sodium chloride.The acetonitrile solution was cleaned up by dispersive solid-phase extraction.The analytes were determined by ultra performance liquid chromatography-tandem mass spectrometry.Factors affecting the extraction efficiency,such as type of extraction solvent,cleanup sorbent and instrumental condition,were investigated.The performance of this method was evaluated under the optimal conditions at the same time.The results indicated that the matrix effects of four target compounds in corn were more than 10％,and the matrix effects of the other three target compounds in soil were more than 10％ except that for the RPA202248 was less than 10％.The calibration curves for all the analytes were linear in the range of 0.001-1.0 μg/mL with correlation coefficients of 0.994 5-0.999 5.The recoveries at spiked range of 0.005-0.1 mg/kg were in the range of 72.9％-116.5％,with relative standard deviations(n =5) of 0.75％-17.8％.The limits of quantitation were 0.005-0.01 mg/kg.With the advantage of quickness,high performance and environmental friendliness,the developed method is suitable for the determination of thiencarbazonemethyl,isoxaflutole and their metabolites residues in corn and soil.