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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 C_(18)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/m L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20μg/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0.50μg/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 liquid chromatography-tandem mass spectrometry (LC-MS / MS) system for the determination of four kinds of nitrofuran drugs in aquatic products. Methods Nitrofuran residues in the sample were extracted with ethyl acetate, dehydrated with anhydrous sodium sulfate, concentrated under reduced pressure, and purified by HLB solid phase extraction column. The residue was separated on a Waters XTerra C_ (18) column using acetonitrile and water as The mobile phase was eluted by gradient elution. The electrospray ionization ion source positive and negative ion switching and multi-reaction selective monitoring mode were used for mass spectrometry analysis and quantified by external standard method. Results The linearity of 4 kinds of nitrofurans in the range of 1 ~ 40 ng / m L was good with the correlation coefficients above 0.999. The average recoveries of furazolidone, furidone, nitrofurazone and nitrofurantoin were between 88.3% and 102% at the levels of 1, 5 and 20 μg / kg, with the coefficients of variation of intra-assay and inter-assay lower than 15%. The detection limits of four kinds of nitrofuran drugs were 0.50μg / kg. Conclusion The method is rapid, accurate and sensitive and can be used to detect the residues of nitrofurans in aquatic products.