液相色谱-同位素稀释串联质谱法测定动物源性食品中硝基呋喃类代谢物残留

Determination of nitrofuran metabolite residues in food of animalorigin by liquid chromatography-isotope dilution tandem mass spectrometry

加入同位素标记物的动物源性样品(龙虾、肠衣),在酸性条件下用2-硝基苯甲醛,使样品中呋喃唑酮、呋喃西林、呋喃它酮、呋喃妥因实现衍生。经乙酸乙酯提取浓缩、用甲醇水溶液溶解过滤后,滤液用液相色谱-串联质谱定量。在0.5,1.0和2.0μg/kg 3个浓度水平上进行添加回收试验,回收率为80.1%～92.2%,检出限(LOQ)均为0.3μg/kg。方法采用多通道监测及同位素稀释技术,无需几种待测物的液相分离即可实现样品中硝基呋喃类代谢物残留的测定。

Four kinds of nitrofuran metabolites in food of animal origin（lobsters and casings） with spiked isotope-marked compounds were derived by 2-nitrobenzaldehyde under acidic conditions.After extracted and concentrated by ethyl acetate,the extract was dissolved in methanol-water and filtered.The filtrate was analyzed by liquid chromatography-tandem mass spectrometry（LC-MS/MS） and quantified by isotope dilution.The recovery experiments were conducted at levels of 0.5,1.0 and 2.0 μg/kg,and the recoveries were 80.1%~92.2%.The limit of quantification was 0.3 μg/kg.With the multi-channel and isotope dilution technology,this method provided determination of nitrofuran metabolite residues in samples without the separation of those target compounds.