QuPPe-超高效液相色谱-串联质谱法测定蔬菜中呋虫胺及其代谢物残留

Simultaneous Determination of Dinotefuran and Its Metabolites in Vegetables by QuPPe-UPLC-MS/MS

建立超高效液相色谱-串联质谱检测蔬菜中呋虫胺及其代谢物1-甲基-3-[(3-四氢呋喃)甲基]二氢胍盐(1-methyl-3-(tetrahydro-3-furylmethyl)guanidium dihydrogen,DN)、1-甲基-3-[(3-四氢呋喃)甲基]脲(1-methyl-3-(tetrahydro-3-furylmethyl)urea,UF)残留的方法。蔬菜样品采用QuPPe分析方法处理后,经BEH-C18超高效液相色谱柱分离,采用电喷雾正离子模式,通过多反应监测方式测定,基质匹配标准曲线外标法定量。结果表明,呋虫胺及其代谢物在1.25～500μg/L的质量浓度范围内线性关系良好,相关系数均大于0.991,方法检出限为0.04～0.66μg/L,定量限为0.13～2.20μg/L。在3个添加水平条件下,呋虫胺及其代谢物DN、UF在黄瓜、番茄、马铃薯、甘蓝4种基质中的添加回收率为72.0%～109.1%,相对标准偏差为1.4%～12.8%,最低添加量均为10μg/kg。基质效应结果显示,呋虫胺及其代谢物大都表现为中等强度基质效应或强基质效应。该方法简单、准确、高效,可用于蔬菜样品中呋虫胺及其代谢物农药残留的快速筛查和定量检测。

A method for the simultaneous identification and quantification of dinotefuran and its metabolites 1-methyl-3-(tetrahydro-3-furylmethyl)guanidium dihydrogen(DN)and 1-methyl-3-(tetrahydro-3-furylmethyl)urea(UF)in vegetables(cucumber,tomato,potato,and cabbage)was developed using quick polar pesticides(QuPPe)extraction procedure combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The analytes were separated on a UPLC BEH-C18 column,detected in the positive ion mode(ESI+)using multiple reaction monitoring(MRM),and quantified by an external standard method.The proposed method showed good linearity in the range of 1.25–500μg/L with regression coefficients of higher than 0.991.The limits of detection(LODs)ranged between 0.04 and 0.66μg/L,and the limits of quantification(LOQs)were between 0.13 and 2.20μg/L.The average recoveries of the analytes from spiked samples of cucumber,tomato,potato,and cabbage(the lowest spiked concentration level was 10μg/kg)were in the range of 72.0%–109.1%with good precisions(relative standard deviation,RSD=1.4%–12.8%).The majority of the analytes exhibited moderate or strong matrix effects.Results suggested that the method is simple,accurate,efficient and useful for rapid screening and quantitative analysis of dinotefuran and its metabolites in vegetables.