Xingyun Zhao , Chengxiao Zhao , Rongfang Wu , Jiangyan Jin , Xiaojian Liu , Zhenwei Zhang , Siyu Yang , Ke Li , Zhenyu Li , Xuemei Qin
{"title":"Synthesis and chromatographic evaluating of the core-shell SiO2 with tunable shell thickness and application for separation of Traditional Chinese Medicine oligosaccharides","authors":"Xingyun Zhao , Chengxiao Zhao , Rongfang Wu , Jiangyan Jin , Xiaojian Liu , Zhenwei Zhang , Siyu Yang , Ke Li , Zhenyu Li , Xuemei Qin","doi":"10.1016/j.chroma.2025.465864","DOIUrl":null,"url":null,"abstract":"<div><div>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 SiO<sub>2</sub> 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 <em>n</em>-octadecyltrichlorosilane modified core-shell silica particles with tunable shell thickness. Column efficiencies up to ∼168, 325 plates m<sup>-1</sup> were achieved for pyrene on the CS<sub>X-E</sub>-C18 column (<em>n</em>-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 CS<sub>X-E</sub>-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.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1748 ","pages":"Article 465864"},"PeriodicalIF":3.8000,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Chromatography A","FirstCategoryId":"1","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0021967325002122","RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
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.
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.