【摘要】 目的建立贝类产品中呋喃唑酮、呋喃它酮、呋喃西林、呋喃妥因和硝夫索尔代谢物的同位素稀释液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)检测方法。方法样品中加入同位素内标,经盐酸水解及邻硝基苯甲醛衍生,调节pH为7.2±0.2,乙酸乙酯提取,氮吹浓缩,正己烷去脂净化,色谱柱分离,电喷雾电离(electronic spray ion, ESI)正负离子多反应(multiple reaction monitoring, MRM)模式检测,同位素内标稀释法定量。结果 5种硝基呋喃代谢物的方法定量限为0.1～0.2μg/kg;方法的线性范围为0.2～20μg/kg;相关系数均大于0.999;方法平均回收率为88.7%～112.1%,相对标准偏差为3.9%～13.7%。应用该方法对280份贝类产品进行检测,其中45份样品中检出了含量较低的氨基脲,范围值在0.21～1.86μg/kg。结论方法灵敏准确,适合贝类产品中硝基呋喃代谢物的检测。更多还原

【Abstract】 Objective To establish an analytical method for determination of furazolidone,furaltadone,nitrofurazone,nitrofurantoin and nifursol metabolites in shellfish by isotope dilution liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods Isotopic internal standards were added to the sample,which then were hydrolyzed by hydrochloric acid and derivatized with 2-nitrobenzaldehyde.The solution was neutralized to pH 7.2±0.2,extracted with ethyl acetate,and evaporated to dryness with nitrogen.The residue was reconstituted with mobile phase,and defatted with acetonitrile saturated n-hexane.The analytes were quantified by LC-MS/MS operating in both positive and negative ion multiple monitoring modes(MRM),and quantitatively determined by isotope internal standard dilution method.Results Limits of quantifications for the 5 nitrofuran metabolites were 0.1-0.2 μg/kg.The matrix calibration curves were established with correlation coefficients more than 0.999 in the range of 0.2-20 μg/kg.The average recoveries were ranged from 88.7% to 112.1%,with the relative standard deviations of 3.9%-13.7%.The method was successfully applied for 280 shellfish products,and 45 of them were confirmed with low levels of semicarbazide(SEM) ranging from 0.21 to 1.86 μg/kg.Conclusion The proposed method has high sensitivity and good accuracy,which is suitable for determination of nitrofuran metabolites in shellfish products.更多还原