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用于开管毛细管电色谱的氧化石墨烯修饰触手型聚合物固定相的制备与表征

Preparation and characterization of tentacle-type polymer stationary phase modified with graphene oxide for open-tubular capillary electrochromatography.

作者信息

Gao Xing, Mo Rongzhen, Ji Yibing

机构信息

Department of Analytical Chemistry, China Pharmaceutical University, Nanjing, China; Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, Nanjing, China.

Department of Analytical Chemistry, China Pharmaceutical University, Nanjing, China; Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, Nanjing, China.

出版信息

J Chromatogr A. 2015 Jun 26;1400:19-26. doi: 10.1016/j.chroma.2015.04.039. Epub 2015 Apr 28.

Abstract

In this research, a novel organic polymer coated stationary phase modified with inorganic nanomaterial was prepared for open-tubular capillary electrochromatography (OT-CEC). The capillary was developed by covalent attaching graphene oxide (GO) onto the tentacle-type polymer chains grafted capillary which was derivatized with ammonium hydroxide. Scanning electron microscopy (SEM) and Raman spectroscopy provided evidences that the tentacle-type polymer and GO were coated to the capillary inner wall. This novel GO-polymer modified capillary column generated a strong and stable electroosmotic flow (EOF) from anode to cathode with the running electrolytes of pH ranging from 4.0 to 9.0, and showed excellent separation ability toward neutral small molecules, amino acids and ephedrine-pseudoephedrine isomers with resolution higher than 2.30 and column efficiency up to over 170,000 plates/m. The repeatabilities of the GO-GMA@capillary were satisfying with relative standard deviations for intra-day and inter-day runs less than 3.27%, and column-to-column runs less than 7.49%. Additionally, the separation performance of GO-polymer modified capillary was compared with that of the polymer coated capillary and GO coated capillary.

摘要

在本研究中,制备了一种用无机纳米材料改性的新型有机聚合物涂层固定相,用于开管毛细管电色谱(OT-CEC)。通过将氧化石墨烯(GO)共价连接到用氢氧化铵衍生化的触手型聚合物链接枝毛细管上,来制备毛细管。扫描电子显微镜(SEM)和拉曼光谱提供了证据,证明触手型聚合物和GO被涂覆到毛细管内壁上。这种新型的GO-聚合物改性毛细管柱在pH值为4.0至9.0的运行电解质中产生了从阳极到阴极的强而稳定的电渗流(EOF),并且对中性小分子、氨基酸和麻黄碱-伪麻黄碱异构体显示出优异的分离能力,分辨率高于2.30,柱效高达170,000塔板数/米以上。GO-GMA@毛细管的重复性令人满意,日内和日间运行的相对标准偏差小于3.27%,柱间运行的相对标准偏差小于7.49%。此外,还将GO-聚合物改性毛细管的分离性能与聚合物涂层毛细管和GO涂层毛细管的分离性能进行了比较。

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