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Net-like mesoporous carbon nanocomposites for magnetic solid-phase extraction of sulfonamides prior to their quantitation by UPLC-HRMS
Microchimica Acta ( IF 5.7 ) Pub Date : 2020-01-09 , DOI: 10.1007/s00604-019-4072-7
Siyuan Di 1 , Jing Yu 1 , Pin Chen 1 , Gangtian Zhu 1 , Shukui Zhu 1
Affiliation  

A net-like mesoporous carbon nanocomposite (MCN) was hydrothermally prepared by using filter paper as the raw material. The MCN contains magnetic nanoparticles of type Fe 3 O 4 which result from the addition of Fe(NO 3 ) 3 ·9H 2 O during synthesis. The MCN was characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, Raman spectra, Brunauer-Emmett-Teller methods and vibrating sample magnetometry. The MCN is shown to be a viable material for magnetic solid-phase extraction of trace sulfonamides (SAs) including sulfadiazine, sulfapyridine, sulfamerazine, sulfamethazine, sulfamethizole, sulfamethoxypridazine, sulfachloropyridazine and sulfadimethoxine. Following desorption with acetone containing 0.5% ammonia, the SAs were quantified by UPLC with high-resolution mass spectrometric detection. With sulfamethazine as an example, the adsorption equilibrium configurations and the major interaction mechanism between SAs and the MCN were calculated by using density functional theory. Under the optimal conditions, the calibration plots are linear in the 0.05–10 ng·mL −1 SA concentration ranges. The limits of detection are between 7.2 and 13.6 ng·L −1 . The recoveries from spiked samples ranged from 79 to 107%, with relative standard deviations of <9.9%. Graphical abstract Schematic representation of nanocomposite preparation, adsorption mechanism of sulfonamide and magnetic solid-phase extraction (MSPE) for sulfadiazine (SDZ), sulfapyridine (SPD), sulfamerazine (SMR), sulfamethazine (SMZ), sulfamethizole (SMT), sulfamethoxypridazine (SMP), sulfachloropyridazine (SCP) and sulfadimethoxine (SDMX). Quantification was accomplished by UPLC with high-resolution mass spectrometric detection

中文翻译:

网状介孔碳纳米复合材料用于磺胺类药物的磁性固相萃取,然后通过 UPLC-HRMS 进行定量

以滤纸为原料,水热法制备了网状介孔碳纳米复合材料(MCN)。MCN包含Fe 3 O 4 型磁性纳米粒子,其由合成过程中添加Fe(NO 3 ) 3 ·9H 2 O产生。MCN 通过 X 射线衍射、傅里叶变换红外光谱、扫描电子显微镜、透射电子显微镜、拉曼光谱、Brunauer-Emmett-Teller 方法和振动样品磁强计进行表征。MCN 被证明是用于痕量磺胺 (SA) 磁性固相萃取的可行材料,包括磺胺嘧啶、磺胺吡啶、磺胺二甲嘧啶、磺胺二甲嘧啶、磺胺二甲嘧啶、磺胺甲氧哒嗪、磺胺氯哒嗪和磺胺二甲氧嘧啶。用含 0.5% 氨的丙酮解吸后,SAs 通过 UPLC 与高分辨率质谱检测进行定量。以磺胺二甲嘧啶为例,利用密度泛函理论计算了SAs与MCN之间的吸附平衡构型和主要相互作用机制。在最佳条件下,校准图在 0.05–10 ng·mL -1 SA 浓度范围内呈线性。检测限在 7.2 和 13.6 ng·L -1 之间。加标样品的回收率范围为 79% 至 107%,相对标准偏差 <9.9%。图形摘要纳米复合材料制备示意图、磺胺吸附机理和磁性固相萃取 (MSPE) 对磺胺嘧啶 (SDZ)、磺胺吡啶 (SPD)、磺胺嘧啶 (SMR)、磺胺二甲嘧啶 (SMZ)、磺胺甲唑 (SMT)、磺胺甲氧嘧啶 (SMP) ), 磺胺氯哒嗪 (SCP) 和磺胺二甲氧嘧啶 (SDMX)。定量是通过 UPLC 与高分辨率质谱检测完成的
更新日期:2020-01-09
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