街头流动餐饮食品中氨基甲酸酯类农药残留的超高效液相色谱-串联质谱检测

Determination of carbamates residues in street food by liquid chromatography-tandem mass spectrometry

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。

In this work, a quantitative method was developed for the simultaneous determination of carbaryl, propoxur and carbofuran in street food by liquid chromatography-tandem mass spectrometry（ LC-MS、MS）. The samples were extracted by acetonitrile, desahed with sodium chloride, and purified by amino solid phase extraction column. Constant volume solvent was the mixture of acetonitrile and 0.1% formic acid（ 1 ∶1, v/v）. Then the sample were separated through Agilent Poroshell120ec-C18 column, and detected by the electrospray ionization tandem mass spectrometry in multi reaction monitoring mode. The method showed a good linear relationship in determination range for three pesticide residues（ r〉0.99）. The limit of detection（ LOD） was0.2-1.0 μg/kg（ S/N=3）. At the standard level of 10, 50 and 100 μg/L, the recoveries were between 76.1% and 90.6%, and the relative standard deviations were 0.25%-6.43%. This method has the advantages of simple pretreatment, short analysis time, good selectivity and the high sensitivity, which is suitable for rapid determination of carbamates residues in street food.