微波辅助衍生-液相色谱-串联质谱法快速测定养殖水体中5种硝基呋喃类代谢物残留

Determination of Nitrofuran Metabolites in Fishery Water by Microwave Assisted Derivatization and Liquid Chromatography-Tandem Mass Spectrometry

建立了微波辅助衍生结合液相色谱-串联质谱（MAD-LC-MS/MS）同时测定水产养殖用水中硝基呋喃类代谢物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）、1-氨基-2-丙酰脲（AHD）和3,5-二硝基水杨酸肼（DNSAH）的分析方法。样品经2-硝基苯甲醛微波辅助衍生1min,乙酸乙酯提取,Acquity UPLC BEH C18色谱柱分离,以乙腈-乙酸铵（5mmol/L,0.1%甲酸）溶液为流动相,梯度洗脱,电喷雾正负离子切换模式电离,多反应监测模式（MRM）测定。结果表明：5种代谢物在0.2～50μg/L范围内线性关系良好,相关系数均大于0.997,方法的定量限为0.02～0.05μg/L;在0.1～5μg/L的3个添加水平下,回收率在79%～102%之间,相对标准偏差（RSD）在3.6%～10.1%之间。该方法快速、简便,且易于推广,可以同时监测养殖水体中5种硝基呋喃代谢物的残留。

A method based on microwave-assisted derivatization（MAD）with liquidchromatography-tandem mass spectrometry（LC-MS/MS）was developed for determination of 3-amino-2-oxazolidinone（AOZ）,3-amino-5-morpholinomethy-2-oxazolidinone（AMOZ）,semicarbazide（SEM）,1-aminohydantoin（AHD）and 3,5-dinitrosalicylic acid hydrazide（DNSAH）in fishery water.The sample was extracted with ethyl acetate,then was derivatized with 2-nitrobenzaldehyde using microwave assisted method for 1min.The analysis was carried out on an Acquity UPLC BEH C18 column by gradient elution with acetonitrile-ammonium acetate（5 mmol/L,0.1% formic acid）as mobile phase,and was detected by LC-MS/MS system with positive and negative electrospray ionization under multiple reaction monitoring（MRM）mode.The results show that the metabolites have good linearity in the range of 0.2-50μg/L,and the correlation coefficients（R2）are better than 0.997.The limits of quantification（LOQs）of the five targets are in the range of 0.02-0.05μg/L.The average recoveries range from 79% to102%for the five targets at three spiked levels with the relative standard deviations of3.6%-10.1%.The method is proved to be fast and effective for simultaneously qualitative and quantitative inspection of the metabolites of nitrofuran in fishery water.