1.2μm新型放射型核壳色谱填料在加压毛细管电色谱中的性能评价

doi:10.3724/SP.J.1123.2015.12039

色谱 ›› 2016, Vol. 34 ›› Issue (5): 461-466.DOI: 10.3724/SP.J.1123.2015.12039

1.2μm新型放射型核壳色谱填料在加压毛细管电色谱中的性能评价

施文君¹, 田华君¹, 薛芸¹, 翁中亚¹, 瞿其曙², 王彦¹, 阎超¹

1. 上海交通大学药学院, 上海 200240;
2. 安徽建筑大学材料与化学工程学院, 安徽合肥 230601

收稿日期:2015-12-31 出版日期:2016-05-08 发布日期:2012-12-18
通讯作者: 阎超, 王彦
基金资助:
国家自然科学基金项目(21175092);上海市科委科研计划项目(15142200200);上海市教育委员会科研创新项目(14YZ170);中国博士后科学基金项目(2015M581628).

Performance evaluation of 1.2 μ m fibrous core-shell packing material for pressurized capillary electrochromatography

SHI Wenjun¹, TIAN Huajun¹, XUE Yun¹, WENG Zhongya¹, QU Qishu², WANG Yan¹, YAN Chao¹

1. School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China;
2. School of Materials and Chemical Engineering, Anhui Jianzhu University, Hefei 230601, China

Received:2015-12-31 Online:2016-05-08 Published:2012-12-18
Supported by:
National Natural Science Foundation of China (No. 21175092); Research and Development Program of Shanghai Municipal Science and Technology Commission (No. 15142200200); Innovation Program of Shanghai Municipal Education Commission (No. 14YZ170); China Postdoctoral Science Foundation Funded Project (No. 2015M581628).

摘要/Abstract

摘要：

研究制备了1.2 μ m放射型核壳色谱填料,并对其表面进行了键合C18的改性,通过匀浆填充法制备了总长度为350 mm(固定相有效填充长度为70 mm)、内径为100 μ m的毛细管色谱柱,应用加压毛细管电色谱(pCEC)法考察了硫脲和萘在该色谱柱上的分离性能,同时讨论了流动相中有机相的比例、缓冲液的浓度、pH值、线性流速及施加电压对分离度的影响。实验结果表明,该新型核壳色谱填料在乙腈水体系中分离硫脲和萘时,表现出典型的反相色谱性能,当含有10 mmol/L磷酸的70%(v/v)乙腈水溶液为流动相、缓冲液pH为7.2、施加电压为-10 kV时,柱效最高;在最佳线性流速为1 mm/s时,能够在8 min内实现8种中性物质的基线分离,且峰形较好,其中二苯甲酮的柱效高达19072块/m。该研究表明1.2 μ m新型放射型核壳色谱填料适用于pCEC法的分离分析。

关键词: 1.2 &mu, m放射型核壳色谱填料, 反相色谱, 加压毛细管电色谱

Abstract:

Silica microsphere packing material with fibrous shells (1.2 μ m) was successfully synthesized and bonded with octadecylsilane functionality. These stationary phase particles were packed into fused-silica capillary with 100 μ m i.d. for a total length of 350 mm (70 mm effective length), which was evaluated for pressurized capillary electrochromatography (pCEC). The efficiency of the C18 reversed-phase column was characterized through the theoretical plates of thiourea and naphthalene. The effects of experimental parameters such as the content of acetonitrile in the mobile phase, the concentration of the buffer solution, the pH value of the mobile phase, the flow rate, the applied voltage and the on-column efficiency were investigated. The results showed a typical reversed-phase chromatographic performance. The eight neutral compounds were baseline separated within 8 min and the column efficiency as high as 190792 plate/m for benzophenone was obtained with the optimal conditions of 10 mmol/L phosphate buffer (pH 7.2) in 70% (v/v) acetonitrile aqueous solution at an applied negative voltage of 10 kV and a supplementary pressure of 1.66×10⁷ Pa. The optimal linear velocity was 1 mm/s. The research work confirmed the feasibility of using 1.2 μ m silica microsphere packing material with fibrous shells as a novel stationary phase for pCEC.

Key words: 1.2 &mu, m fibrous core-shell packing material, pressurized capillary electrochromatography (pCEC), reversed phase chromatography

中图分类号:

O658

施文君, 田华君, 薛芸, 翁中亚, 瞿其曙, 王彦, 阎超. 1.2μm新型放射型核壳色谱填料在加压毛细管电色谱中的性能评价[J]. 色谱, 2016, 34(5): 461-466.

SHI Wenjun, TIAN Huajun, XUE Yun, WENG Zhongya, QU Qishu, WANG Yan, YAN Chao. Performance evaluation of 1.2 μ m fibrous core-shell packing material for pressurized capillary electrochromatography[J]. Chinese Journal of Chromatography, 2016, 34(5): 461-466.

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1.2μm新型放射型核壳色谱填料在加压毛细管电色谱中的性能评价

Performance evaluation of 1.2 μ m fibrous core-shell packing material for pressurized capillary electrochromatography

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