Determination of fluoroquinolones in fishes using microwave-assisted extraction combined with ultra-high performance liquid chromatography and fluorescence detection
Determination of fluoroquinolones in fishes using microwave-assisted extraction combined with ultra-high performance liquid chromatography and fluorescence detection
复制标题
DOI：
10.1016/j.jfca.2016.12.012
复制
发表时间：
2017-03-01
影响因子：
4.3
通讯作者：
Santana-Rodriguez, J. J.
中科院分区：
文献类型：
--
作者：
Aufartova, J.;Brabcova, I.;Santana-Rodriguez, J. J.
建立了一种基于超高效液相色谱-荧光检测（UHPLC-FD）的水产养殖用氟喹诺酮类抗生素（诺氟沙星、环丙沙星、恩诺沙星、达诺沙星和萨拉沙星）在鱼类肌肉（如金头鲷）中的含量测定方法。采用微波辅助萃取(MAE) -净化预浓缩-固相萃取(SPE) - UHPLC-FD检测相结合的方法进行提取和测定。通过实验设计，研究了不同因素对MAE-SPE的影响。根据决议2002/657/EC进行验证。根据最大残留限量（MRL）测定CC α和CC β。方法的检出限（MDL）在0.1 ~ 6.0 ng g（-1）之间。在25和250 ng g（-1）两种加标浓度下，加标回收率均大于90%，相对标准偏差小于8.7%。所开发的方法已成功地应用于评价在大加那利岛（西班牙）各商业商店购买的水产养殖场的鱼肌肉样品中FQs的存在。(C) 2016 Elsevier Inc.版权所有。
A new analytical methodology based on ultra-high performance liquid chromatography with fluorescence detection (UHPLC-FD) has been developed for the determination of five fluoroquinolone antibiotics (FQs) used in aquaculture (norfloxacin, ciprofloxacin, enrofloxacin, danofloxacin and sarafloxacin) in fish muscles (e.g. gilthead seabream (Sparus aurata)). The extraction and determination process was carried out by combining microwave-assisted extraction (MAE) along with a clean-up and pre-concentration step with solid phase extraction (SPE) followed by UHPLC-FD detection. The effects of different variables on MAE-SPE were studied and optimized using an experimental design. Validation was made in accordance with Decision 2002/657/EC. CC alpha and CC beta were determined according to the maximum residue limit (MRL). The method detection limit (MDL) of the entire process ranged between 0.1 and 6.0 ng g(-1). The recoveries obtained at two spiked concentrations levels (25 and 250 ng g(-1)) were greater than 90%, and the relative standard deviation was less than 8.7%. The developed methodology was successfully applied for the evaluation of the presence of FQs in fish muscle samples from aquaculture farms bought in various commercial shops in Gran Canaria Island (Spain). (C) 2016 Elsevier Inc. All rights reserved.