IF 3.8 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS
Xingyun Zhao , Chengxiao Zhao , Rongfang Wu , Jiangyan Jin , Xiaojian Liu , Zhenwei Zhang , Siyu Yang , Ke Li , Zhenyu Li , Xuemei Qin
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引用次数: 0

摘要

开发核壳材料以实现更高效、更快速的色谱分离一直是分离科学的关键目标。本研究利用单分散 SiO2 颗粒(直径为 2-4 µm),通过改良溶胶-凝胶工艺和双相系统相结合的方法制造核壳球体。合成采用了 1,6-双(三乙氧基硅基)己烷(BTMSH)、1,2-双(三乙氧基硅基)乙烷(BTEE)作为架桥剂,十六烷基三甲基溴化铵(CTAB)作为辅助模板。值得注意的是,通过对搅拌速率、溶剂选择和二氧化硅前驱体类型进行系统优化,可以在 70 ∼ 300 nm 的范围内精确定制外壳厚度。对芳烃分析物的分离情况进行了评估,结果表明,在所有填装了正十八烷基三氯硅烷修饰的核壳二氧化硅颗粒、且壳厚度可调的色谱柱上,两种分子都实现了基线分离。在 CSX-E-C18 色谱柱(正十八烷基三氯硅烷改性核壳硅胶)上,芘的色谱柱分离效率高达 ∼168, 325 plates m-1。此外,还通过改进的聚合涂层方法制备了一种亲水相互作用液相色谱(HILIC)核壳固定相,即酰胺修饰的核壳白炭黑(命名为 CSX-E-AM),并将其应用于低聚糖的分离。结果表明,所制备的核壳球体具有定制的壳体结构,而且柱子稳定,能满足高效液相色谱分离的要求。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Synthesis and chromatographic evaluating of the core-shell SiO2 with tunable shell thickness and application for separation of Traditional Chinese Medicine oligosaccharides
The development of core-shell materials for achieving more efficient and rapid chromatographic separations has remained a key objective in separation science. In this study, monodisperse SiO2 particles (2–4 µm in diameter) were utilized to fabricate core-shell spheres through a combined approach involving a modified sol-gel process and a biphasic system. The synthesis employed 1,6-bis(triethoxysilyl) hexane (BTMSH), 1,2-bis(triethoxysilyl) ethane (BTEE) as a bridging agent with cetyltrimethylammonium bromide (CTAB) acting as a co-template. Notably, the shell thickness could be precisely tailored within the range of 70∼300 nm through systematic optimization of stirring rate, solvent selection, and silica precursor type. The separation of aromatics analytes was evaluated and that baseline separation was achieved for both molecules on all the columns packed n-octadecyltrichlorosilane modified core-shell silica particles with tunable shell thickness. Column efficiencies up to ∼168, 325 plates m-1 were achieved for pyrene on the CSX-E-C18 column (n-octadecyltrichlorosilane modified core-shell silica). In addition, a hydrophilic interaction liquid chromatography (HILIC) core-shell stationary phase that amide modified core shell silica was prepared (named as CSX-E-AM) via an improved polymerization coating approach and applied for oligosaccharides separation. The results demonstrated that the core-shell spheres were prepared with tailored shell structure and exhibited that the column was stable and could meet the requirement for HPLC separation.
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来源期刊
Journal of Chromatography A
Journal of Chromatography A 化学-分析化学
CiteScore
7.90
自引率
14.60%
发文量
742
审稿时长
45 days
期刊介绍: The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.
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