液相色谱-串联质谱法检测水产品中硝基呋喃类药物的残留量

摘要

目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)检测水产品中4种硝基呋喃类药物的残留量.方法 样品中残留的硝基呋喃类药物经乙酸乙酯提取,无水硫酸钠脱水,减压浓缩后过HLB固相萃取柱净化,经Waters XTerra C18色谱柱分离,采用乙腈和水作为流动相进行梯度洗脱,以电喷雾离子源正负离子切换和多反应选择监测模式进行质谱分析,以外标法定量.结果 4种硝基呋喃类药物在1～40 ng/mL范围内线性关系良好,相关系数均大于0.999.在添加水平为1、5和20 μg/kg时,呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因的平均回收率在88.3％～102％之间,批内和批间变异系数均低于15％.4种硝基呋喃类药物的检出限均为0.50 μg/kg.结论 该方法快速、准确、灵敏,可满足水产品中硝基呋喃类药物残留量的检测.%Objective To establish a method for simultaneous determination of four kinds of nitrofurans residues in aquatic products by liquid chromatography-tandem mass spectrometry (LC-MS/MS).Methods The residues of nitrofurans in samples were extracted with ethyl acetate,and dehydrated with anhydrous sodium sulfate.Then the extracts were concentrated in vacuum condition,and purified on HLB solid phase extraction column.The residues of nitrofurans in the extracts were separated by Waters XTerra C18 column using acetonitrile and ultrapure water as mobile phase for gradient elution.Electrospray ionization was applied and operated in positive and negative ion switching mode with multiple reactions monitoring (MRM) for mass analysis with external standard method for quantification.Results The calibration curves were good linear between area and the concentration of four kinds of nitrofurans in the ranges of 1～40 ng/mL with the correlation coefficients all above 0.999.The recoveries of furazolidone,nitrofurazone,furaltadone and furantoin were ranged from 88.3％ to 102％,with spiked at levels of 1,5 and 20 μg/kg.The intra and inter batch relative standard deviations were less than 15％.The detection limits of four kinds ofnitrofurans were all 0.50 μg/kg.Conclusion The established method is rapid,accurate and efficient,which can be used to identify and quantify the four nitrofurans in aquatic products.