Heparin/heparan sulfate analysis by covalently modified reverse polarity capillary zone electrophoresis-mass spectrometry.
Heparin/heparan sulfate analysis by covalently modified reverse polarity capillary zone electrophoresis-mass spectrometry.
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DOI：
10.1016/j.chroma.2018.02.052
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发表时间：
2018-04-13
期刊：
影响因子：
--
通讯作者：
Amster IJ
中科院分区：
文献类型：
--
作者：
Sanderson P;Stickney M;Leach FE 3rd;Xia Q;Yu Y;Zhang F;Linhardt RJ;Amster IJ
反极性毛细管区带电泳-负离子模式质谱（CZE-MS）联用技术是分析糖胺聚糖混合物的有效和灵敏的工具。用中性或阳离子试剂对分离毛细管的内壁进行共价改性，产生稳定且耐用的表面，从而提供可再现的分离。将CZE-MS与阳离子涂层毛细管和鞘流接口相结合，建立了一种快速、可靠的分析硫酸寡糖dp 4-dp 12的方法。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分辨结构中的细微差异的能力，例如硫酸化位置和糖醛酸的差向异构体变化。该系统被施加到一个复杂的混合物肝素/硫酸乙酰肝素低聚糖不同的链长从DP 3到DP 12和超过80个分子组合物被确定通过准确的质量测量。
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.
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