硫醇-烯点击化学法制备C<sub>18</sub>毛细管电色谱开管柱及其性能研究

引用本文: 陈霞, 韦誉, 陆俊宇, 张爱珠, 叶芳贵, 赵书林. 硫醇-烯点击化学法制备C₁₈毛细管电色谱开管柱及其性能研究[J]. 分析化学, 2012, 40(10): 1584-1588. doi: 10.3724/SP.J.1096.2012.20329 shu

Citation: CHEN Xia, WEI Yu, LU Jun-Yu, ZHANG Ai-Zhu, YE Fang-Gui, ZHAO Shu-Lin. Preparation and Evaluation of C₁₈ Modified Capillary Open-tubular Column Based on Thiol-ene Click Chemistry for Capillary Electrochromatography[J]. Chinese Journal of Analytical Chemistry, 2012, 40(10): 1584-1588. doi: 10.3724/SP.J.1096.2012.20329 shu

硫醇-烯点击化学法制备C₁₈毛细管电色谱开管柱及其性能研究

通讯作者: 叶芳贵

基金项目:
本文系国家自然科学基金(No.21065002) (No.21065002)

广西自然科学基金(No.2012GXNSFAA053024) (No.2012GXNSFAA053024)

广西壮族自治区研究生教育创新计划(No.2011106020703M47)资助 (No.2011106020703M47)

摘要: 基于十八烷基硫醇与乙烯基功能化毛细管(Vinyl capillary)的硫醇-烯点击化学反应, 制备了一种新型的C₁₈毛细管电色谱开管柱(C₁₈ capillary)。采用乙烯基三甲氧基硅烷对毛细管内壁进行乙烯基功能化,然后通过硫醇-烯点击化学反应共价键合十八烷基硫醇于Vinyl capillary内表面。采用环境扫描电镜对C₁₈ capillary进行了形貌表征。考察了缓冲溶液pH值对C₁₈ capillary、Vinyl capillary和裸毛细管柱(Bare capillary)电渗流的影响。结果表明;在相同实验条件下,C₁₈ capillary的电渗流最小。以3种多环芳烃为模型化合物,评价了C₁₈ capillary的电色谱柱性能;同时考察了模型化合物在C₁₈ capillary上的电色谱保留行为。实验表明,其保留机理是基于典型的反相作用。当C₁₈ capillary用于碱性模型化合物分离时,碱性物质在C₁₈ capillary上的峰形较好,无明显的峰拖尾现象,这可能是由于C₁₈ capillary 表面含有极性的S基团能够屏蔽残留硅羟基对碱性化合物的吸附作用。

关键词:

English

Preparation and Evaluation of C₁₈ Modified Capillary Open-tubular Column Based on Thiol-ene Click Chemistry for Capillary Electrochromatography

1.
Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources, Ministry of Education of China, College of Chemistry & Chemical Engineering of Guangxi Normal University, Guilin 541004, China

Corresponding author: 叶芳贵

Received Date: 28 March 2012
Fund Project:
本文系国家自然科学基金(No.21065002)

广西自然科学基金(No.2012GXNSFAA053024)

广西壮族自治区研究生教育创新计划(No.2011106020703M47)资助

Abstract: A novel C₁₈ open-tubular column (C₁₈ capillary) for capillary electrochromatography was prepared based on thiol-ene click chemistry between n-octadecanethiol and vinyl-functionalized capillary (Vinyl capillary). The inner wall of capillary was chemically modified with vinyltrimethoxysilane to provide ene-functionality. Then n-octadecanethiol was chemically bonded on surface of Vinyl capillary via thiol-ene click chemistry. The surface features of the prepared C₁₈ capillary were determined using scanning electron microscopy. The effects of buffer pH on the electroosmotic flow (EOF) of C₁₈ capillary, Vinyl capillary and bare capillary were investigated. The experiment results indicated that the lowest EOF profile was obtained on the C₁₈ capillary under the same experimental conditions compared to Vinyl capillary and bare capillary. To evaluate the column performance, test mixture of three polycyclic aromatic hydrocarbons (PAHs) was electrochromatographic separation on the C₁₈ capillary, Vinyl capillary and bare capillary. The electrochromatographic retention behavior of the selected model PAHs on C₁₈ capillary was also investigated. The experiment results showed that C₁₈ capillary exhibited typical reversed phase electrochromatographic behavior toward PAHs. Compared with Vinyl capillary, the relatively good peak shape and no peak tailing were observed for the separation of basic model analytes on C₁₈ capillary, which may be attributed to embedded polar sulphur groups on the surface of the C₁₈ capillary that effectively shielded the adsorption of basic analytes onto the residual silanol groups.

Key words:

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

硫醇-烯点击化学法制备C₁₈毛细管电色谱开管柱及其性能研究

通讯作者: 叶芳贵

English

Preparation and Evaluation of C₁₈ Modified Capillary Open-tubular Column Based on Thiol-ene Click Chemistry for Capillary Electrochromatography

Corresponding author: 叶芳贵

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通讯作者: 陈斌, bchen63@163.com

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硫醇-烯点击化学法制备C18毛细管电色谱开管柱及其性能研究

通讯作者: 叶芳贵

English

Preparation and Evaluation of C18 Modified Capillary Open-tubular Column Based on Thiol-ene Click Chemistry for Capillary Electrochromatography

Corresponding author: 叶芳贵

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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