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A hollow porous molecularly imprinted polymer as a sorbent for the extraction of 7 macrolide antibiotics prior to their determination by HPLC-MS/MS
Microchimica Acta ( IF 5.7 ) Pub Date : 2018-03-01 , DOI: 10.1007/s00604-018-2728-3
Shunli Ji , Tengfei Li , Wen Yang , Chang Shu , Duo Li , Yan Wang , Li Ding

AbstractA hollow porous molecularly imprinted polymer (HPMIP) is described for use in dispersive solid phase extraction of macrolide antibiotics (MACs). The HPMIP was prepared by using spiramycin as the template, methacrylic acid as the functional monomer, and mesoporous MCM-41 (Mobile Composition of Matter No. 41; with a size of about 100 nm) as a sacrificial support. The sorbent was characterized by Fourier transform infrared spectrometry, transmission electron microscopy, nitrogen adsorption and thermo-gravimetric analysis. Several parameters affecting the extraction efficiency were optimized. The material has a large surface area (359 m2·g−1), and most recognition sites are located on the surface of the HPMIPs. This results in high binding capacity (120 μmol·g−1) and fast binding (20 min) in comparison to either MCM-41-core surface MIPs or solid MIPs. The method was applied to the extraction of the MACs azithromycin, spiramycin, tilmicosin, tylosin, clarithromycin, roxithromycin and josamycin from spiked honey. The recoveries, determined by HPLC-MS/MS, ranged from 88.0% to 117% at the three spiking levels tested (1, 5 and 20 μg·kg−1). Intra-day and inter-day assay precision at three spiking levels are <10.7% (for n = 6) and 12.6% (n = 3), respectively. The limits of detection are between 3 and 17 ng·kg−1. This indicates the superiority of the method in selective extraction of macrolides even from complex matrices. Graphical abstractHollow porous molecularly imprinted polymers using spiramycin as the template are shown to be viable dispersive solid phase extraction adsorbents for selective enrichment of macrolide antibiotics in honey products prior to their quantitation by HPLC-MS/MS.

中文翻译:

中空多孔分子印迹聚合物作为吸附剂,用于在 HPLC-MS/MS 测定之前提取 7 种大环内酯类抗生素

摘要描述了一种中空多孔分子印迹聚合物 (HPMIP),用于大环内酯类抗生素 (MAC) 的分散固相萃取。以螺旋霉素为模板,甲基丙烯酸为功能单体,介孔MCM-41(Movement Composition of Matter No.41;尺寸约100 nm)为牺牲载体制备HPMIP。通过傅里叶变换红外光谱、透射电子显微镜、氮吸附和热重分析对吸附剂进行了表征。对影响提取效率的几个参数进行了优化。该材料具有较大的表面积(359 m2·g-1),大多数识别位点位于 HPMIP 的表面。与 MCM-41 核心表面 MIP 或固体 MIP 相比,这导致高结合容量 (120 μmol·g-1) 和快速结合 (20 分钟)。该方法用于从加标蜂蜜中提取MACs中的阿奇霉素、螺旋霉素、替米考星、泰乐菌素、克拉霉素、罗红霉素和交沙霉素。通过 HPLC-MS/MS 测定的回收率在三个测试的加标水平(1、5 和 20 μg·kg-1)下为 88.0% 至 117%。三个加标水平的日内和日间测定精度分别为 <10.7%(n = 6)和 12.6%(n = 3)。检测限在 3 到 17 ng·kg-1 之间。这表明该方法在从复杂基质中选择性提取大环内酯方面的优越性。
更新日期:2018-03-01
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