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基于超高效液相色谱-高分辨质谱联用技术的实际水产品中恩诺沙星及其代谢物的残留筛查与分析。

Residue screening and analysis of enrofloxacin and its metabolites in real aquatic products based on ultrahigh-performance liquid chromatography coupled with high resolution mass spectrometry.

机构信息

State Key Laboratory of Analytical Chemistry for Life Science, School of Chemistry & Chemical Engineering and Center of Materials Analysis, Nanjing University, Nanjing 210023, China.

Jiangsu Institute for Food and Drug Control, 6 Beijing West Road, Nanjing 210008, China.

出版信息

Food Chem. 2023 Mar 15;404(Pt B):134757. doi: 10.1016/j.foodchem.2022.134757. Epub 2022 Oct 28.

Abstract

The abuse of enrofloxacin (ENR) in aquaculture and the lack of monitoring of other metabolites except ciprofloxacin (CIP) may lead to unknown harmful effects on human health. In this study, ENR metabolites were screened in real fish samples based on ultrahigh-performance liquid chromatography coupled with Q-Orbitrap mass spectrometry combined with Compound Discoverer software, and another metabolite deethylene-ENR besides CIP was detected and identified for the first time. Correspondingly, a method for the determination of ENR and CIP and the semi-quantitative analysis of deethylene-ENR in aquatic products was established. Method validation illustrated that excellent linearity and satisfactory recoveries of analytes were obtained. Limits of detection of ENR and CIP were both 0.1 μg kg, and their limits of quantification both 1 μg kg. CIP and deethylene-ENR were detected in 12 of 14 ENR-positive fish samples, so deethylene-ENR should be of concern as a possible risk candidate in aquatic products.

摘要

恩诺沙星(ENR)在水产养殖中的滥用以及除环丙沙星(CIP)以外的其他代谢物监测的缺乏,可能对人类健康造成未知的有害影响。在本研究中,基于超高效液相色谱与 Q-Orbitrap 质谱联用结合 Compound Discoverer 软件,在真实的鱼类样本中筛选了 ENR 代谢物,首次检测并鉴定出除 CIP 以外的另一种代谢物去乙烯基-ENR。相应地,建立了水产品中 ENR 和 CIP 的测定方法以及去乙烯基-ENR 的半定量分析方法。方法验证表明,分析物具有良好的线性和令人满意的回收率。ENR 和 CIP 的检测限均为 0.1μgkg,定量限均为 1μgkg。在 14 个 ENR 阳性鱼类样本中有 12 个检测到了 CIP 和去乙烯基-ENR,因此去乙烯基-ENR 应该被视为水产品中可能的风险候选物。

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