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Heparin/heparan sulfate analysis by covalently modified reverse polarity capillary zone electrophoresis-mass spectrometry.
Journal of Chromatography A ( IF 4.1 ) 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:

肝素/硫酸乙酰肝素的共价修饰反极性毛细管区带电泳-质谱分析。

反相毛细管区带电泳与负离子模式质谱分析(CZE-MS)结合使用,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的内壁进行共价修饰,可形成稳定耐用的表面,从而提供可重复的分离效果。通过将CZE-MS与带阳离子涂层的毛细管和鞘流界面相结合,已开发出一种快速而可靠的方法,用于分析dp4至dp12中的硫酸化寡糖。几种不同的混合物已被分离并通过质谱检测。选择混合物以测试该方法解决结构上细微差异的能力,例如硫酸化位置和糖醛酸的差向异构体变化。

更新日期:2018-02-24
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