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通过深共晶溶剂优化杂原子掺杂氧化石墨烯及其在黄酮类化合物的微量进样固相萃取中的应用。

Optimization of heteroatom doped graphene oxide by deep eutectic solvents and the application for pipette-tip solid-phase extraction of flavonoids.

机构信息

Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin, P. R. China.

出版信息

J Sep Sci. 2019 Jul;42(14):2371-2378. doi: 10.1002/jssc.201900317. Epub 2019 Jun 26.

Abstract

In order to improve the permeation and adsorption properties of graphene oxide, heteroatoms and deep eutectic solvent were introduced in this study. After being modified, the structural properties of graphene oxide were improved and the materials were applied to the determination of myricetin and rutin in tea sample by pipette-tip solid-phase extraction method. The materials were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, X-Ray diffractomer, energy dispersive spectroscopy, atomic force microscope, and specific surface area by Brunauer-Emmett-Teller N adsorption desorption analysis. Meanwhile, they were tested by static and dynamic adsorption. The result showed that the materials after modifying had better adsorption amount for myricetin and rutin than graphene oxide. The calibration graphs of myricetin and rutin in MeOH were linear over 0.10-500.00 µg/mL, and the limits of detection and quantification were in the range of 0.00546-0.0182 µg/mL and 0.00741-0.0247 µg/mL, respectively. A reliable analytical method was developed for recognition targets in tea sample by DES modified nitrogen-doped graphene oxide with satisfactory extraction recoveries (myricetin 99.77%, rutin 98.14%). It was potential for the rapid purification of myricetin and rutin in tea sample combined with the pipette-tip solid-phase extraction.

摘要

为了提高氧化石墨烯的渗透和吸附性能,本研究引入了杂原子和深共晶溶剂。经过修饰后,氧化石墨烯的结构性能得到了改善,并将材料应用于茶样中杨梅素和芦丁的测定,采用微量进样固相萃取法。通过扫描电子显微镜、傅里叶变换红外光谱、X 射线衍射仪、能量色散光谱、原子力显微镜和 Brunauer-Emmett-Teller N 吸附解吸分析对材料进行了表征。同时,对其进行了静态和动态吸附测试。结果表明,修饰后的材料对杨梅素和芦丁的吸附量均优于氧化石墨烯。杨梅素和芦丁在 MeOH 中的校准曲线在 0.10-500.00 µg/mL 范围内呈线性,检出限和定量限分别为 0.00546-0.0182 µg/mL 和 0.00741-0.0247 µg/mL。建立了一种用 DES 修饰氮掺杂石墨烯氧化还原法测定茶样中识别物的可靠分析方法,杨梅素的提取回收率为 99.77%,芦丁的提取回收率为 98.14%。结合微量进样固相萃取,该方法有望快速纯化茶样中的杨梅素和芦丁。

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