【摘要】 目的建立水产品中呋喃它酮、呋喃西林、呋喃妥因和呋喃唑酮等硝基呋喃代谢物的固相萃取-高效液相色谱-串联质谱测定方法。方法样品中加入同位素内标,经盐酸水解及2-硝基苯甲醛衍生,再经Oasis HLB固相萃取小柱净化,乙酸乙酯洗脱吹氮浓缩;采用XTerraMS C18色谱分离柱,以乙腈-5 mmol/L乙酸铵的0.1%甲酸水溶液进行梯度洗脱,以正离子多反应监测模式,同位素内标法定量。结果 4种硝基呋喃代谢物的定量限为0.10～0.30μg/kg;方法的线性范围为0.5～25μg/kg,r>0.995;代谢衍生物的加标回收率分别为81.0%～104.8%、91.0%～110.3%、85.0%～111.4%和88.0%～108.2%;RSD在2.7%～14.5%之间。应用建立的方法对180份淡水鱼进行测定,其中4份检出3-氨基-2-噁唑烷基酮(AOZ),含量为1.3～3.6μg/kg。结论方法选择性高、灵敏,能满足水产品中硝基呋喃类代谢物残留的高灵敏分析。更多还原

【Abstract】 Objective The method for determination of metabolites of four nitrofuran antibiotics,nitrofurantoin(AMOZ),furaltadone(SEM),nitrofurazone(AHD) and furazolidone(AOZ) in aquatic products was developed by solid-phase extraction coupled with liquid chromatography tandem mass spectrometry(LC-MS/MS).Methods Samples with isotope internal standard solutions were hydrolyzed by HCl and derivatized with 2-nitrobenzaldehyde.The analytes were cleaned up on HLB solid-phase column and eluted with ethyl acetate,then evaporated and dried with nitrogen gas.The extract components were separated and gradient eluted on a XTerra C18 column with acetonitrile-5 mmol/L ammonium acetate of 0.1% formic acid solutions ion,and simultaneously quantified by the isotope internal standard operating in positive ion under multiple reactions monitoring mode.Results The limits of quantification ranged from 0.10 μg/kg to 0.30 μg/kg for four nitrofuran metabolites.The standard curves were linear in the range of 0.5-25 μg/kg,with the correlation coefficients>0.995.The average recoveries for nitrofuran metabolites were 81.0%-104.8%,91.0%-110.3%,85.0%-111.4%,88.0%-108.2% respectively,and their relative standard deviation varied between 2.7% and 14.5%.The method was applied to analyze 180 fish samples from Guangdong region,four of which were confirmed to contain AOZ ranging from 1.3 to 3.6 μg/kg.Conclusion The method developed was selective,sensitive and accurate,completely suitable for nitrofuran metabolites trace analysis in aquatic products.更多还原