Citation: 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. doi: 10.3724/SP.J.1123.2015.12039 shu

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

SHI Wenjun ¹ ,
TIAN Huajun ¹ ,
XUE Yun ¹ ,
WENG Zhongya ¹ ,
QU Qishu ² ,
WANG Yan ^1,, ,
YAN Chao ^1,,

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

Corresponding author: WANG Yan, YAN Chao,
Received Date: 31 December 2015

Fund Project: 国家自然科学基金项目(21175092) (21175092)上海市科委科研计划项目(15142200200) (15142200200)上海市教育委员会科研创新项目(14YZ170) (14YZ170)中国博士后科学基金项目(2015M581628). (2015M581628)

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.
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