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Heparin/heparan sulfate analysis by covalently modified reverse polarity capillary zone electrophoresis-mass spectrometry.
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2018-02-24 , DOI: 10.1016/j.chroma.2018.02.052
Patience Sanderson 1 , Morgan Stickney 1 , Franklin E Leach 1 , Qiangwei Xia 2 , Yanlei Yu 3 , Fuming Zhang 3 , Robert J Linhardt 3 , I Jonathan Amster 1
Affiliation  

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.



中文翻译:


通过共价修饰反极性毛细管区带电泳-质谱法进行肝素/硫酸乙酰肝素分析。



反极性毛细管区带电泳与负离子模式质谱 (CZE-MS) 联用被证明是分析糖胺聚糖混合物的有效且灵敏的工具。用中性或阳离子试剂对分离毛细管内壁进行共价修饰,产生稳定耐用的表面,从而提供可重复的分离。通过将 CZE-MS 与阳离子涂层毛细管和鞘流接口相结合,开发了一种快速可靠的方法,用于分析从 dp4 到 dp12 的硫酸化寡糖。几种不同的混合物已被分离并通过质谱法检测。选择混合物来测试该方法解决结构中细微差异的能力,例如糖醛酸的硫酸化位置和差向异构变化。该系统应用于链长从 dp3 到 dp12 的肝素/硫酸乙酰肝素低聚糖的复杂混合物,并通过精确质量测量鉴定了 80 多种分子组成。

更新日期:2018-02-24
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