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磁性 N 掺杂 3D 类石墨烯骨架碳用于提取头孢氨苄一水合物和头孢噻呋盐酸盐。

Magnetic N-doped 3D graphene-like framework carbon for extraction of cephalexin monohydrate and ceftiofur hydrochloride.

机构信息

CAS Key Laboratory of Chemistry of Northwestern Plant Resource and Key Laboratory for Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou, Gansu, 730000, PR China; University of Chinese Academy of Sciences, Beijing, 100049, PR China.

Research Institute of Experiment and Detection of Xinjiang Oilfield Company, Karamay, Xinjiang, 834000, PR China.

出版信息

Talanta. 2020 Aug 1;215:120932. doi: 10.1016/j.talanta.2020.120932. Epub 2020 Mar 17.

Abstract

Magnetic N-doped 3D graphene-like framework carbon (FeO@N-3DFC) was prepared via direct pyrolysis of sodium citrate and further hydrothermal reaction, and employed in the extraction of two cephalosporin antibiotics including cephalexin monohydrate and ceftiofur hydrochloride. The scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectrometry, X-ray photoelectron spectroscopy and X-ray diffraction were employed to confirm the successful synthesis of 3DFC-based adsorbents (3DFCs) including 3DFC, FeO@3DFC and FeO@N-3DFC. FeO@N-3DFC sorbent with 3D graphene-like honeycomb architecture combined magnetic and N doping shows the attractive features including graphene carbon sheets, hierarchical porous structure, good wettability and higher surface affinity for cephalosporin antibiotics. Furthermore, the comparison of extraction efficiency with raw 3DFC and FeO@3DFC sorbent also confirmed the superiority of FeO@N-3DFC sorbent. Under optimized conditions, good linearity lines were obtained with the determination coefficients from 0.9953 to 0.9995. The limit of detections were in the range of 0.20-0.45 μg L and 0.03-0.10 μg L for cephalexin and ceftiofur, respectively. The spiked extraction recoveries were between 81.59% and 98.35% with the relative standard deviation values less than 6.98%. Combined with high performance liquid chromatography, FeO@N-3DFC based magnetic solid-phase extraction was successfully applied in river water and zebrafish samples analysis.

摘要

通过柠檬酸钠的直接热解和进一步的水热反应,制备了磁性 N 掺杂 3D 类石墨烯骨架碳(FeO@N-3DFC),并将其用于提取两种头孢菌素抗生素,包括头孢氨苄一水合物和盐酸头孢噻呋。扫描电子显微镜、透射电子显微镜、傅里叶变换红外光谱、X 射线光电子能谱和 X 射线衍射用于确认 3DFC 基吸附剂(3DFCs)的成功合成,包括 3DFC、FeO@3DFC 和 FeO@N-3DFC。具有 3D 类石墨烯蜂窝结构的 FeO@N-3DFC 吸附剂结合了磁性和 N 掺杂,具有吸引人的特点,包括石墨烯碳片、分层多孔结构、良好的润湿性和对头孢菌素抗生素更高的表面亲和力。此外,与原始 3DFC 和 FeO@3DFC 吸附剂的萃取效率比较也证实了 FeO@N-3DFC 吸附剂的优越性。在优化条件下,头孢氨苄和头孢噻呋的检测系数分别在 0.9953 至 0.9995 之间,检测限在 0.20 至 0.45μg/L 和 0.03 至 0.10μg/L 之间。头孢氨苄和头孢噻呋的加标萃取回收率在 81.59%至 98.35%之间,相对标准偏差值小于 6.98%。结合高效液相色谱法,FeO@N-3DFC 基磁性固相萃取成功应用于河水和斑马鱼样品分析。

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