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超高效液相色谱-串联质谱法测定水产品中硝基呋喃代谢物残留量

Determination of nitrofurans metabolites residues in aquatic products by ultra-performance liquid chromatography-tandem mass spectrometry.

作者信息

Zhang Yibei, Qiao Haiou, Chen Chen, Wang Zhilun, Xia Xiaodong

机构信息

College of Food Science and Engineering, Northwest A&F University, Yangling, Shaanxi 712100, PR China.

Shaanxi Provincial Center for Disease Control and Prevention, Xi'an, Shaanxi 710054, PR China.

出版信息

Food Chem. 2016 Feb 1;192:612-7. doi: 10.1016/j.foodchem.2015.07.035. Epub 2015 Jul 9.

Abstract

A method was described for monitoring four nitrofuran metabolites including 5-methylmorpholino-3-amino-2-oxazolidinone (AMOZ), 3-amino-2-oxazolidone (AOZ), 1-amino-hydantoin (AHD) and semicarbazide (SEM) in aquatic products. The analytes were quantified by ultra-performance liquid chromatography-tandem mass spectrometry operating in positive ion multiple monitoring mode (MRM) after 2-nitrobenzaldehyde derivatization. The matrix calibration curve was established with correlation coefficient (R(2)>0.99) in the range of 1-100 ng ml(-1). Limit of detection and limit of quantification for all analytes were 0.5 and 1.5 μg kg(-1), respectively. Recovery rates and relative standard deviations ranged from 88% to 112% and 2% to 4%, respectively. The validated method was successfully applied to detect nitrofuran metabolites in 120 fish samples. The analytes were detected in 6/16 species of fish samples, with a total detection rate of 6.5%. AOZ was most frequently detected (8.3%), followed by AMOZ (7.5%), AHD (5.0%) and SEM (5.0%). The method is proposed for monitoring nitrofuran metabolites in aquatic products.

摘要

本文描述了一种监测水产品中四种硝基呋喃代谢物的方法,这四种代谢物包括5-甲基吗啉基-3-氨基-2-恶唑烷酮(AMOZ)、3-氨基-2-恶唑烷酮(AOZ)、1-氨基乙内酰脲(AHD)和氨基脲(SEM)。在2-硝基苯甲醛衍生化后,采用超高效液相色谱-串联质谱法在正离子多反应监测模式(MRM)下对分析物进行定量。基质校准曲线在1-100 ng ml(-1)范围内建立,相关系数(R(2)>0.99)。所有分析物的检测限和定量限分别为0.5和1.5 μg kg(-1)。回收率和相对标准偏差分别为88%至112%和2%至4%。该验证方法成功应用于120份鱼样品中硝基呋喃代谢物的检测。在16种鱼类样品中有6种检测到了分析物,总检出率为6.5%。AOZ的检出频率最高(8.3%),其次是AMOZ(7.5%)、AHD(5.0%)和SEM(5.0%)。该方法可用于监测水产品中的硝基呋喃代谢物。

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