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聚乙烯亚胺功能化 FeO/凹凸棒土颗粒用于亲水作用磁性分散固相萃取鸡肉肌肉中的氟喹诺酮类药物。

Polyethyleneimine-functionalized FeO/attapulgite particles for hydrophilic interaction-based magnetic dispersive solid-phase extraction of fluoroquinolones in chicken muscle.

机构信息

School of Materials and Chemical Engineering, Ningbo University of Technology, Ningbo, 315211, China.

Ningbo Academy of Inspection and Quarantine, Ningbo, 315012, China.

出版信息

Anal Bioanal Chem. 2021 May;413(13):3529-3540. doi: 10.1007/s00216-021-03304-9. Epub 2021 Apr 4.

Abstract

Fluoroquinolone (FQ) residues in foods of animal origin may threaten public health but are challenging to determine because of their low contents and complex matrices. In this study, novel polyethyleneimine-functionalized FeO/attapulgite magnetic particles were prepared by a simple co-mixing method and applied as hydrophilic sorbents for the magnetic dispersive solid-phase extraction (MSPE) of three FQs, i.e., ciprofloxacin, norfloxacin, and enrofloxacin, from chicken muscle samples. The preparation of the magnetic particles was of high reproducibility and the products could be reused many times with high adsorption capacity. The key experimental factors possibly influencing the extraction efficiencies, including sample solution, extraction time, sample loading volume, desorption solution, desorption time, and elution volume were investigated. Under optimum MSPE conditions, the analytes in chicken muscle samples were extracted and then determined by RPLC-MS/MS in MRM mode. Good linearity was obtained for the analytes with correlation coefficients ranged from 0.9975 to 0.9995. The limits of detection were in the range of 0.02-0.08 μg kg, and the recoveries of the spiked FQs in chicken muscle samples ranged from 83.9 to 98.7% with relative standard deviations of 1.3-6.8% (n = 3). Compared with the traditional MSPE methods based on hydrophobic mechanism, this hydrophilic interaction-based method significantly simplifies the sample pretreatment procedure and improves repeatability. This method is promising for accurate monitoring of FQs in foods of animal origin.

摘要

动物源食品中的氟喹诺酮(FQ)残留可能会威胁到公众健康,但由于其含量低且基质复杂,因此难以检测。在本研究中,通过简单的共混法制备了新型的聚乙烯亚胺功能化 FeO/凹凸棒石磁性粒子,并将其用作亲水吸附剂,用于从鸡肉样品中磁性分散固相萃取(MSPE)三种 FQs,即环丙沙星、诺氟沙星和恩诺沙星。磁性粒子的制备具有很好的重现性,并且可以多次重复使用,具有很高的吸附能力。研究了可能影响萃取效率的关键实验因素,包括样品溶液、萃取时间、样品加载体积、解吸溶液、解吸时间和洗脱体积。在最佳 MSPE 条件下,鸡肉样品中的分析物通过 RPLC-MS/MS 在 MRM 模式下进行提取和测定。分析物在 0.02-0.08 μg kg 范围内具有良好的线性关系,相关系数范围为 0.9975-0.9995。在鸡肉样品中的 FQs 加标回收率为 83.9-98.7%,相对标准偏差为 1.3-6.8%(n=3)。与基于疏水机制的传统 MSPE 方法相比,这种基于亲水相互作用的方法显著简化了样品预处理步骤,提高了重复性。该方法有望用于准确监测动物源食品中的 FQs。

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