色谱

色谱 ›› 2015, Vol. 33 ›› Issue (9): 922-928.DOI: 10.3724/SP.J.1123.2015.03028

• 亲水作用色谱专栏 • 上一篇    下一篇

叠氮基修饰硅胶固定相在亲水模式下的色谱评价及应用(英文)

赵艳艳1, 李秀玲2, 郭志谋2, 梁鑫淼2   

  1. 1. 大连医科大学药学院, 辽宁 大连 116044;
    2. 中国科学院分离分析化学重点实验室, 中国科学院大连化学物理研究所, 辽宁 大连 116023
  • 收稿日期:2015-03-23 出版日期:2015-09-08 发布日期:2015-09-09
  • 通讯作者: 李秀玲
  • 基金资助:

    National Natural Science Foundation of China (Nos. 21105100, 21105007, 21475129) and the Dalian Science and Technology Project, China (No. 2012E15SF145).

Chromatographic evaluation and application of silica based azide-modified stationary phase under hydrophilic interaction liquid chromatography mode

ZHAO Yanyan1, LI Xiuling2, GUO Zhimou2, LIANG Xinmiao2   

  1. 1. Pharmacy College, Dalian Medical University, Dalian 116044, China;
    2. Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
  • Received:2015-03-23 Online:2015-09-08 Published:2015-09-09
  • Supported by:

    National Natural Science Foundation of China (Nos. 21105100, 21105007, 21475129) and the Dalian Science and Technology Project, China (No. 2012E15SF145).

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摘要：

亲水作用液相色谱(HILIC)近年来引起了越来越多的关注,然而用于亲水液相色谱的固定相种类仍然有限,需要开发更多的固定相和分离分析方法。我们课题组开发和评价了基于硅胶基质的叠氮基固定相。首先,采用核苷作为测试样品对固定相的保留性质进行了评价,结果表明核苷在叠氮基固定相上的保留符合亲水液相色谱的典型特征。其次,比较了亲水模式下流动相中两种缓冲盐(碳酸氢铵和甲酸铵)和酸添加剂对叠氮基固定相糖肽富集选择性的影响。结果表明当流动相中不加缓冲盐并且调成酸性时,糖肽富集选择性更高,在优化富集条件后,从辣根过氧化物酶(HRP)中富集得到9条糖肽信号,所开发的叠氮基固定相具有在HILIC模式下使用的广阔前景。

关键词: 叠氮基修饰的硅胶固定相, 亲水液相色谱, 糖肽富集

Abstract:

Hydrophilic interaction liquid chromatography (HILIC) has attracted more and more interests in recent years. However, the stationary phases for HILIC are still scarce. More stationary phases and separation methods should be developed. Silica based azide-modified stationary phase was synthesized and characterized by our group. The nucleosides were selected as the test samples. The retention property of nucleosides on the azide-modified stationary phase was shown with typical HILIC characterization. Moreover, the glycopeptide selectivities of azide-modified stationary phase under HILIC mode by adding two species of salts (ammonium bicarbonate and ammonium formate) and acid in mobile phase were compared. The results showed that better glycopeptide selectivity could be obtained under acid condition without adding salt in the mobile phase. With the optimized conditions, nine MS signals of glycopeptides were detected after enrichment from the tryptic digest of horseradish peroxidase (HRP). Silica based azide-modified stationary phase has the potential in further application in glycopeptide enrichment under HILIC mode.

Key words: glycopeptide enrichment, hydrophilic interaction liquid chromatography (HILIC), silica based azide-modified stationary phase

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