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目的建立了超高效液相色谱-串联质谱法定量测定街头流动餐饮食品中甲萘威、残杀威、克百威3种氨基甲酸酯类混合农药残留的方法。样品经乙腈提取,氯化钠盐析分层,氨基固相萃取小柱净化,以乙腈-0.1%甲酸水(1:1,v/v)为定容溶剂,经Agilent Poroshell120ec-C18色谱柱分离,电喷雾串联质谱多反应监测模式测定。3种化合物在测定的范围内线性关系良好(r>0.99),方法的检出限为0.2~1.0μg/kg(S/N=3)。在加标水平为10、50、100μg/L时,方法的回收率为76.1%~90.6%,相对标准偏差为0.25%~6.43%。该方法样品前处理简单,分析时间短,选择性好,灵敏度高,适用于街头流动餐饮食品中氨基甲酸酯类农药的快速测定。
OBJECTIVE To establish a method for the quantitative determination of carbaryl, carbofuran and carbofuran carbamate residues in street food products by ultra performance liquid chromatography-tandem mass spectrometry. The samples were separated by acetonitrile, salted-sodium chloride and purified by amino-solid phase cartridge. The sample was separated on an Agilent Poroshell 120ec-C18 column with acetonitrile-0.1% formic acid water (1: 1, v / v) , Electrospray ionization tandem mass spectrometry multiple reaction monitoring mode determination. The three compounds showed good linearity (r> 0.99) within the limits of determination. The detection limit of the method was 0.2-1.0 μg / kg (S / N = 3). The method recoveries ranged from 76.1% to 90.6% and the relative standard deviations (RSDs) ranged from 0.25% to 6.43% at spiked levels of 10, 50 and 100 μg / L. The method has the advantages of simple sample preparation, short analysis time, good selectivity and high sensitivity, and is suitable for the rapid determination of carbamate pesticides in street food products.