超高效液相色谱-串联质谱法测定烤鳗中硝基呋喃类代谢物残留量

Determination of residues of nitrofurans in roasted eel by ultra performance liquid chromatography-tandem mass spectrometry

目的：建立用超高效液相色谱-串联质谱（UPLC-MS-MS）测定烤鳗中3-氨基-2-唑烷基酮（AOZ）、5-甲基吗啉-3-氨基-2-唑烷基酮（AMOZ）、氨基脲（SEM）和1-氨基-2-内酰脲（AHD）4种硝基呋喃类代谢物的定性、定量分析方法。方法：先用甲醇/水（1：1）混洗烤鳗肉组织,去掉大量杂质,用0.25 mol/L盐酸水解组织中蛋白结合代谢物,经2-硝基苯甲醛衍生化,乙酸乙酯提取后,采用电喷雾电离,正离子扫描,多反应监测（MRM）模式检测,内标法定量。结果：4种硝基呋喃代谢物的定量限均能达到0.5μg/kg。在0.5-10 ng/g浓度范围内,4种硝基呋喃类代谢物的工作曲线均呈良好线性,相关系数r〉0.99,回收率为77%-111%,相对标准偏差在7.52%-16.59%。结论：本方 法快速、简便、准确、灵敏度高且经济,适用于烤鳗中硝基呋喃类代谢物的确证和定量分析。

Objective：To develop a method based on ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） for the determination of low-level residues of four nitrofurans including 3-amino-2-oxazolidinone（AOZ）,semicarbazide（SEM）,5-methylmorpholino-3-amino-2-oxazolidinone（AMOZ） and 1-amino-hydantoin（AHD） in roasted eel muscles.Methods：Using methanol/H2O（1：1） to remove any soluble matters,roasted eel samples were hydrolyzed with 0.25 mol/L HCl,and derivatized at 37℃ for 16 h with 2-nitrobenzaldenhyde.The target compounds were eluted with ethyl acetate from the derivatized solutions,and finally diluted with mobile phase.MS detection was performed in the positive ion mode using multiple reaction monitoring（MRM）.The quantification was obtained ultilizing the homologous internal standards.Results：The limits of detection were 0.5 μg/kg for all the four nitrofurans.The standard curves were linear in the range of added concentration between 0.5~10 μg/kg,with the corelation coefficients 〉0.99.The recovery rates were 77%~111% and the RSD were 7.52%~16.59%.Conclusion：This method is rapid,simple,precise,sensitive and economical for both confirmation and quantification of nitrofurans in roasted eel.