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高分辨质谱筛查法在检测受损鱼类和进口养殖样本中兽药残留的应用与评估

Application and evaluation of a high-resolution mass spectrometry screening method for veterinary drug residues in incurred fish and imported aquaculture samples.

机构信息

US Food and Drug Administration, Animal Drugs Research Center, Denver, CO, 80225, USA.

US Food and Drug Administration, Center for Veterinary Medicine, 8301 Muirkirk Rd., Laurel, MD, 20708, USA.

出版信息

Anal Bioanal Chem. 2018 Sep;410(22):5529-5544. doi: 10.1007/s00216-018-0917-x. Epub 2018 Feb 14.

Abstract

The ability to detect chemical contaminants, including veterinary drug residues in animal products such as fish, is an important example of food safety analysis. In this paper, a liquid chromatography high-resolution mass spectrometry (LC-HRMS) screening method using a quadrupole-Orbitrap instrument was applied to the analysis of veterinary drug residues in incurred tissues from aquacultured channel catfish, rainbow trout, and Atlantic salmon and imported aquacultured products including European eel, yellow croaker, and tilapia. Compared to traditional MS methods, the use of HRMS with nontargeted data acquisition and exact mass measurement capability greatly increased the scope of compounds that could be monitored simultaneously. The fish samples were prepared for analysis using a simple efficient procedure that consisted of an acidic acetonitrile extraction followed by solid phase extraction cleanup. Two different HRMS acquisition programs were used to analyze the fish extracts. This method detected and identified veterinary drugs including quinolones, fluoroquinolones, avermectins, dyes, and aminopenicillins at residue levels in fish that had been dosed with those compounds. A metabolite of amoxicillin, amoxicillin diketone, was also found at high levels in catfish, trout, and salmon. The method was also used to characterize drug residues in imported fish. In addition to confirming findings of fluoroquinolone and sulfonamide residues that were found by traditional targeted MS methods, several new compounds including 2-amino mebendazole in eel and ofloxacin in croaker were detected and identified. Graphical Abstract Aquacultured samples are analyzed with a high-resolution mass spectrometry screening method to detect and identify unusual veterinary drug residues including ofloxacin in an imported fish.

摘要

检测化学污染物的能力,包括鱼类等动物产品中的兽药残留,是食品安全分析的一个重要例子。在本文中,应用了一种基于四极杆轨道阱仪器的液相色谱-高分辨质谱(LC-HRMS)筛选方法,用于分析养殖斑点叉尾鮰、虹鳟和大西洋三文鱼以及进口养殖产品(包括欧鳗、大黄鱼和罗非鱼)中发生组织的兽药残留。与传统的 MS 方法相比,使用具有非靶向数据采集和精确质量测量能力的 HRMS 极大地增加了可以同时监测的化合物范围。采用一种简单有效的程序对鱼样进行分析,该程序包括酸性乙腈提取,然后进行固相萃取净化。使用两种不同的 HRMS 采集程序分析鱼提取物。该方法可检测并鉴定出喹诺酮类、氟喹诺酮类、阿维菌素类、染料和氨基青霉素类等药物,这些药物在已用这些化合物处理过的鱼类中的残留水平。在鲶鱼、鳜鱼和三文鱼中也发现了阿莫西林的代谢产物阿莫西林二酮。该方法还用于分析进口鱼类中的药物残留。除了通过传统的靶向 MS 方法确认氟喹诺酮类和磺胺类残留的发现外,还检测并鉴定了几种新的化合物,包括鳗鱼中的 2-氨基甲苯咪唑和大黄鱼中的氧氟沙星。

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