高效液相色谱串联质谱法快速测定水产品中硝基呋喃类代谢物研究

建立了一种液相色谱串联质谱方法快速检测水产品中呋喃唑酮代谢物3-氨基-2-唑烷基酮(AOZ)、呋喃它酮代谢物5-甲基吗啉-3-氨基-2-唑烷基酮(AMOZ)、呋喃西林代谢物氨基脲(SEM)、呋喃妥因代谢物1-氨基-乙丙酰脲(AHD)等硝基呋喃类代谢物。样品在40℃水浴超声下经盐酸水解、邻硝基苯甲醛快速衍生化、乙酸乙酯提取、浓缩净化后,采用HPLC-ESI-MS/MS检测分析,在多反应监测模式(MRM)下,外标法定量。以乙腈-0.05%甲酸水为流动相,采用梯度洗脱,30 min内可将4种硝基呋喃代谢物分离。在0.25～25μg/kg范围内标准曲线的相关系数大于0.998。在不同添加水平下的回收率为81.9%～111.6%,定量限(LOQ)为1μg/kg,检出限(LOD)为0.25μg/kg。该方法准确、灵敏,达到了检测水产品中的硝基呋喃类代谢物的要求。

Study on Quick Determination of Nitrofuran Metabolites in Aquatic Products by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

A quick determination method has been developed for the analysis of four nitrofuran metabolites (5-methyl-morpholino-3-amino-2-oxazolidinone,3-amino-2-oxazolidinone,semicarbazide and 1-amino-hydantoin) in aquatic products by liquid chromatography-electrospray ionization tandem mass spectrometry.Samples were hydrolyzed with dilute hydrochloric acid,derivatied with 2-nitrobenzene formaldehyde,extracted by ethyl acetate,then cleaned up,and ultimately adopted LC-ESI-MS/MS method for qualitative and quantitative analysis.Four nitrofuran metabolites could be seperated with a gradient of acetonitrile and 0.05% formic acid in 30 mintues.The calibration graphs were linear from 0.25 to 25 μg/kg,and correlation coefficients >0.998.The average recoveries were from 81.9% to 111.6% in different spike levels.Limits of quantification(LOQ)and limits of detection(LOD)were 1 μg/kg and 0.25 μg/kg.It is concluded that the method is simple,efficient,sensitive,accurate and can meet the requirements of determination for nitrofuran metabolites in aquatic products.