色谱

色谱 ›› 2017, Vol. 35 ›› Issue (5): 473-481.DOI: 10.3724/SP.J.1123.2017.01025

• 研究论文 • 上一篇    下一篇

AAPBA@KCC-1的合成及其对血清中唾液酸和神经节苷脂的分析应用

田华君, 薛芸, 陈巧梅, 王彦, 阎超   

  1. 上海交通大学药学院, 上海 200240
  • 收稿日期:2017-01-20 出版日期:2017-05-08 发布日期:2013-08-28
  • 通讯作者: 王彦,E-mail:wangyan11@sjtu.edu.cn;阎超,E-mail:chaoyan@sjtu.edu.cn.
  • 基金资助:

    上海市科委科研计划项目（15142200200,16142200300）；中国博士后科学基金（2015M581628）；上海市引进技术的吸收与创新专项（XC-ZXSJ-02-2016-11）.

Synthesis of AAPBA@KCC-1 and its application in the analysis of sialic acid and gangliosides in serum

TIAN Huajun, XUE Yun, CHEN Qiaomei, WANG Yan, YAN Chao   

  1. School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China
  • Received:2017-01-20 Online:2017-05-08 Published:2013-08-28
  • Supported by:

    Shanghai Science and Technology Commission Scientific Research Project (Nos. 15142200200, 16142200300); China Postdoctoral Science Fund (No. 2015M581628); Special Fund of Shanghai Introduction of Technology Adsorption and Innovation (No. XC-ZXSJ-02-2016-11).

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摘要：

将3-丙烯酰胺基苯硼酸（AAPBA）修饰在介孔二氧化硅KCC-1的表面，合成AAPBA@KCC-1材料，并通过扫描电子显微镜、透射电子显微镜、N2吸附解吸附测试和X射线光电子能谱对其进行表征；将AAPBA@KCC-1材料作为分散固相萃取（dSPE）的吸附剂，对血清样品中的唾液酸和神经节苷脂（GLS）进行提取和富集；采用傅里叶变换离子回旋共振质谱法和超高效液相色谱-离子淌度-四极杆飞行时间质谱法分别对AAPBA@KCC-1材料吸附得到的唾液酸和神经节苷脂进行分析。结果表明，AAPBA@KCC-1材料能够有效吸附唾液酸和神经节苷脂，简化了样品前处理的操作，可以进一步应用于生物样品中唾液酸和神经节苷脂的研究。

关键词: N-乙酰神经氨酸, 3-丙烯酰胺基苯硼酸, 分散固相萃取, 介孔二氧化硅KCC-1, 神经节苷脂, 唾液酸

Abstract:

A new material AAPBA@KCC-1 was synthesized by using 3-acrylamidophenylboronic acid (AAPBA) modified on mesoporous silica KCC-1. First, AAPBA was modified on the surface of KCC-1 by three-step synthesis method. Then, AAPBA@KCC-1 was characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), N2 adsorption-desorption isotherm and X-ray photoelectron spectroscopy (XPS). AAPBA@KCC-1 was used as the dispersive solid-phase extraction (dSPE) adsorbent to extract and enrich sialic acid and ganglioside (GLS) from serum samples. Finally, Fourier transform ion cyclotron resonance mass spectrometry (FT-MS) and ultra performance liquid chromatography-ion mobility spectrometry-quadrupole time of flight mass spectrometry (UPLC-IMS-QTOF MS) were used to evaluated the adsorption ability of AAPBA@KCC-1 to sialic acid and GLS, respectively. The results showed that AAPBA@KCC-1 can effectively adsorb sialic acid and GLS, and can be used for further studies of sialic acid and GLS in biological samples.

Key words: N-acetylneuraminic acid (Neu5Ac), 3-acrylamidophenylboronic acid (AAPBA), dispersive solid-phase extraction (dSPE), ganglioside (GLS), mesoporous silica KCC-1, sialic acid

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