液相色谱-串联质谱法同时检测蔬菜中克百威和3-羟基克百威残留

Simultaneous determination of carbofuran and 3-hydroxycarbofuran residues in vegetables by liquid chromatography-tandem mass spectrometry

目的建立一种克百威及3-羟基克百威农药残留的液相色谱-串联质谱(liquid chromatographytandem mass spectrometry,LC-MS/MS)检测方法。方法样品经乙腈提取,氯化钠盐析除水后,过氨基固相萃取柱净化,甲醇和二氯甲烷混合溶液洗脱。采用0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱,质谱(ESI+)采用多离子检测模式(MRM)对定量离子和定性离子进行监测。结果本方法在15 min内完成2种目标化合物的分离分析。克百威和3-羟基克百威在10、30和100μg/kg添加水平的回收率为72.0%~106.4%,相对标准偏差小于6.9%(n=6),方法定量限为10μg/kg。结论该方法快速、准确、灵敏,适合测定蔬菜中克百威及3-羟基克百威药物残留。

Objective To establish a method for Simultaneous determination of carbofuran and 3-hydroxycarbofuran residues in vegetable samples by liquid chromatography-tandem mass spectrometric （LC-MS/MS）.Methods Vegetable samples were extracted with acetonitrile,and water was removed after salting out by sodium chloride.And then carbofuran and 3-hydroxycarbofuran residues in the extracts were separated on an amino solid phase extraction column using a gradient elution program of 0.1% formic acid aqueous solution （A） and 0.1% formic acid in acetonitrile solution （B）.Using LC-MS/MS （ESI＋） with multiple reactions monitoring （MRM）,identification of the major components of the residues was performed based upon the intensities of fragments.Results The established method could separate and analyze the two target compounds within 15 min.The recoveries were ranged from 72.0% to 106.4% for the 2 residues with 3 spiked levels of 10,30 and 100 μg/kg.The relative standard deviations （RSDs） were less than 6.9% （n=6）,and the limits of quantitation （LOQ） for the 2 residues were 10 μg/kg.Conclusion The proposed method is rapid,accurate and sensitive,which is suitable for detecting carbofuran and 3-hydroxycarbofuran residues in vegetable samples.