中文摘要：

目的建立一种采用液相色谱-串联质谱法检测水产品中硝呋索尔代谢物残留量的测定方法。方法样品中以结合态形式残留的硝呋索尔代谢物3,5-二硝基水杨酸肼（DNSAH）经盐酸水解,2-硝基苯甲醛衍生,用乙腈提取,以电喷雾离子源负离子扫描模式进行质谱分析,内标法定量。结果 DNSAH在0.2-20μg/L范围内线性关系良好,相关系数r^2〉0.999。DNSAH添加水平为0.50-5.00μg/kg时,平均回收率在88.3%-100%之间,批内和批间变异系数均〈15%。DNSAH的检出限为0.20μg/kg。结论本方法灵敏、高效、简单、重现性好,满足水产品中硝呋索尔代谢物残留量的检测。

英文摘要：

Objective To establish a method for the determination of nifursol metabolites in aquatic products by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.Methods The residue of nifursol metabolite of 3,5-dinitrosaIicyIic acid hydrazide（DNSAH） in sample was hydrolyzed with HCI,and derivatized with nitrobenzaldehyde.Then the analyte was extracted with acetonitrile and then analyzed by HPLC-MS/MS with internal standard method.Electrospray ionization was applied and operated in the negative ion mode.Results The calibration curve had a good linearity between area and the concentration of DNSAH of 0.2-20μg/L with the correlation coefficient over 0.999.The average recoveries from spiked sample at three concentrations of 0.50,2.00 and 5.00 μg/kg were ranged from 88.3%to 100%with intra and inter batch relative standard deviations below 15%.The detection limit of DNSAH was 0.20 μg/kg.Conclusion The efficient and simple method can be used to identify and quantify the nifursol metabolites in aquatic products with satisfactory sensitivity and repeatability.