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肝素/硫酸乙酰肝素的共价修饰反相毛细管区带电泳-质谱分析。

Heparin/heparan sulfate analysis by covalently modified reverse polarity capillary zone electrophoresis-mass spectrometry.

机构信息

Department of Chemistry, University of Georgia, Athens, GA 30602, United States.

760 Parkside Avenue, STE 211, CMP Scientific, Corp., Brooklyn, NY, 11226, United States.

出版信息

J Chromatogr A. 2018 Apr 13;1545:75-83. doi: 10.1016/j.chroma.2018.02.052. Epub 2018 Feb 24.

DOI:10.1016/j.chroma.2018.02.052
PMID:29501428
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC5862776/
Abstract

Reverse polarity capillary zone electrophoresis coupled to negative ion mode mass spectrometry (CZE-MS) is shown to be an effective and sensitive tool for the analysis of glycosaminoglycan mixtures. Covalent modification of the inner wall of the separation capillary with neutral or cationic reagents produces a stable and durable surface that provides reproducible separations. By combining CZE-MS with a cation-coated capillary and a sheath flow interface, a rapid and reliable method has been developed for the analysis of sulfated oligosaccharides from dp4 to dp12. Several different mixtures have been separated and detected by mass spectrometry. The mixtures were selected to test the capability of this approach to resolve subtle differences in structure, such as sulfation position and epimeric variation of the uronic acid. The system was applied to a complex mixture of heparin/heparan sulfate oligosaccharides varying in chain length from dp3 to dp12 and more than 80 molecular compositions were identified by accurate mass measurement.

摘要

反向极性毛细管区带电泳与负离子模式质谱联用(CZE-MS)被证明是分析糖胺聚糖混合物的有效且敏感的工具。通过将中性或阳离子试剂共价修饰分离毛细管的内壁,可以得到稳定且耐用的表面,从而提供可重复的分离。通过将 CZE-MS 与涂有阳离子的毛细管和鞘流接口相结合,已经开发出一种快速可靠的方法来分析 dp4 到 dp12 的硫酸化低聚糖。通过质谱法对几种不同的混合物进行了分离和检测。选择这些混合物来测试该方法解析结构细微差异的能力,例如磺酸基位置和糖醛酸的差向异构体变化。该系统应用于肝素/硫酸乙酰肝素低聚糖的复杂混合物,其链长从 dp3 到 dp12 不等,通过精确质量测量鉴定了 80 多种以上的分子组成。

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