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A graphene oxide surface–molecularly imprinted polymer as a dispersive solid-phase extraction adsorbent for the determination of cefadroxil in water samples

机译:氧化石墨烯表面分子印迹聚合物作为分散固相萃取吸附剂,用于测定水中样品中的头孢氨苄

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In this work, a graphene oxide (GO)–functionalized molecularly imprinted polymer (MIP) (GO–MIPs) was prepared using a non-covalent molecular imprinting approach and applied to dispersive solid-phase extraction (DSPE) coupled with ultra-high-performance liquid chromatography with photodiode array detection (UPLC-PDA) to sensitively detect cefadroxil (FAD) in aqueous solution. FAD was used as a template to synthesize GO–MIPs, with 2-(trifluoromethyl) acrylic acid (TFMAA) and ethylene glycol dimethacrylate (EGDMA) as the monomer and cross-linker, respectively, in methanol. The GO–MIPs was eluted with acetic acid–methanol (20/80, v/v) and then characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermal gravimetric analysis (TGA) and Raman spectroscopy. The selectivity of the GO–MIPs versus a graphene oxide–functionalized non-imprinted polymer (GO–NIPs) was confirmed based on the selectivity factors (SFs) using cefixime, cefoxitin sodium and ceftiofur hydrochloride as structural analogues of FAD. The efficiency of the synthesized GO–MIPs was evaluated through application of the proposed DSPE procedure. The influencing factors of DSPE, such as the sample pH, extraction time, desorption reagents and desorption time, were optimized, and the analytical performance of the developed DSPE-UPLC-PDA method was evaluated under the optimized conditions. Good linearity was obtained over 0.04–6.0 μg mL?1 (R2 = 0.9979), with a detection limit (S/N = 3) of 0.01 μg mL?1. Finally, the developed method was applied to determine the concentration of FAD in water samples, and the spiked average recoveries ranged between 72.5% and 104.8%. The GO–MIPs served as good carriers for the selective adsorption of FAD and showed promise for the preconcentration of FAD in complex samples.
机译:在这项工作中,使用非共价分子印迹方法制备了由氧化石墨烯(GO)官能化的分子印迹聚合物(MIP)(GO-MIPs),并将其应用于分散固相萃取(DSPE)和超高纯高效液相色谱仪,带有光电二极管阵列检测器(UPLC-PDA),可灵敏地检测水溶液中的头孢羟氨苄(FAD)。 FAD用作合成GO-MIP的模板,其中2-(三氟甲基)丙烯酸(TFMAA)和乙二醇二甲基丙烯酸酯(EGDMA)在甲醇中分别作为单体和交联剂。 GO-MIPs用乙酸-甲醇(20/80,v / v)洗脱,然后通过扫描电子显微镜(SEM),透射电子显微镜(TEM),热重分析(TGA)和拉曼光谱进行表征。使用头孢克肟,头孢西丁钠和头孢噻呋盐酸盐作为结构类似物,根据选择性因子(SFs)确定了GO-MIP对石墨烯官能化的非印迹聚合物(GO-NIPs)的选择性FAD。通过应用建议的DSPE程序评估了合成GO-MIP的效率。优化了样品pH,萃取时间,脱附试剂,脱附时间等DSPE的影响因素,并在优化条件下评价了所开发DSPE-UPLC-PDA方法的分析性能。在0.04–6.0μgmL ?1 R 2 = 0.9979),检出限(S / N = 3)为0.01μgmL ?1 。最后,采用改进的方法测定水样中FAD的浓度,加标平均回收率在72.5%至104.8%之间。 GO-MIPs可作为FAD选择性吸附的良好载体,并有望在复杂样品中对FAD进行预浓缩。

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