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十八烷基胺衍生碳点的合成及其在反相/亲水作用液相色谱中的应用。

Synthesis of octadecylamine-derived carbon dots and application in reversed phase/hydrophilic interaction liquid chromatography.

机构信息

College of Chemistry and Pharmaceutical Sciences, Qingdao Agricultural University, No. 700, Changcheng Road, Chengyang District, Qingdao 266109, China.

College of Food Science and Engineering, Qingdao Agricultural University, Qingdao 266109, China.

出版信息

J Chromatogr A. 2021 Oct 25;1656:462548. doi: 10.1016/j.chroma.2021.462548. Epub 2021 Sep 10.

Abstract

In order to make up for the deficiencies of traditional C18 column for separating strong polar compounds, combined with the good hydrophilicity of carbon dots (CDs), novel octadecylamine-derived CDs denoted as C18-CDs are designed, synthesized and applied in RPLC/HILIC mixed-mode chromatography with good separation performance towards both hydrophobic and hydrophilic compounds. C18-CDs are synthesized by simple one-step solvothermal method using octadecylamine and citric acid as carbon sources, and C18-CDs with proper polarity are collected through column chromatography purification. This C18-CDs decorated silica column showed good separation performance for polycyclic aromatic hydrocarbons and alkylbenzenes under RPLC mode. Hydrophilic compounds including sulfonamides, nucleosides and nucleobases also achieved good resolution in HILIC mode. Hydrophobic and π-π stacking interactions play major retaining roles in RPLC, whereas hydrophilic partitioning and hydrogen bond interactions turn to the main retention interactions under HILIC mode. This C18-CDs/SiO column was applied for the fast detection of chloramphenicol in milk without complex sample pretreatment process. Quantitative relationship between the peak area and the concentration of chloramphenicol was established with linear equation of A = 1677c + 173. Satisfactory spiked recoveries in the range of 94.1-109.0% were obtained. This work not only proposes a simple method for improving the polarity of C18 column through forming octadecane into CDs, but also provides novel CDs with certain hydrophobicity/hydrophily suitable for mixed-mode chromatography.

摘要

为了弥补传统 C18 柱分离强极性化合物的不足,结合碳点(CDs)的良好亲水性,设计、合成了新型十八烷基胺衍生的 CDs,并将其应用于反相高效液相色谱/亲水相互作用色谱混合模式中,对疏水性和亲水性化合物均具有良好的分离性能。C18-CDs 通过简单的一步溶剂热法以十八烷基胺和柠檬酸为碳源合成,并通过柱色谱纯化收集具有适当极性的 C18-CDs。这种 C18-CDs 修饰的硅胶柱在反相模式下对多环芳烃和烷基苯表现出良好的分离性能。亲水化合物,包括磺胺类、核苷和碱基,在亲水相互作用色谱模式下也实现了良好的分辨率。疏水和π-π堆积相互作用在反相模式下起主要保留作用,而亲水分配和氢键相互作用在亲水相互作用模式下成为主要保留相互作用。该 C18-CDs/SiO 柱应用于牛奶中氯霉素的快速检测,无需复杂的样品预处理过程。建立了峰面积与氯霉素浓度之间的定量关系,线性方程为 A = 1677c + 173。在 94.1-109.0%的范围内获得了令人满意的加标回收率。这项工作不仅提出了一种通过将十八烷形成 CD 来提高 C18 柱极性的简单方法,而且还提供了具有一定疏水性/亲水性的新型 CD,适用于混合模式色谱。

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