采用液相色谱-质谱联用技术分析肝素中含3-O-磺酸基团的肝素四糖。
Analysis of 3-O-sulfo group-containing heparin tetrasaccharides in heparin by liquid chromatography-mass spectrometry.
作者信息
Li Guoyun, Yang Bo, Li Lingyun, Zhang Fuming, Xue Changhu, Linhardt Robert J
机构信息
College of Food Science and Technology, Ocean University of China, Qingdao, Shandong 266003, China; Department of Chemistry and Chemical Biology, Rensselaer Polytechnic Institute, Troy, NY 12180, USA.
Department of Chemistry and Chemical Biology, Rensselaer Polytechnic Institute, Troy, NY 12180, USA.
出版信息
Anal Biochem. 2014 Jun 15;455:3-9. doi: 10.1016/j.ab.2014.02.033. Epub 2014 Mar 28.
Abstract
Complete heparin digestion with heparin lyase 2 affords a mixture of disaccharides and resistant tetrasaccharides with 3-O-sulfo group-containing glucosamine residues at their reducing ends. Quantitative online liquid chromatography-mass spectrometric analysis of these resistant tetrasaccharides is described in this article. The disaccharide and tetrasaccharide compositions of seven porcine intestinal heparins and five low-molecular-weight heparins were analyzed by this method. These resistant tetrasaccharides account for from 5.3 to 7.3wt% of heparin and from 6.2 to 8.3wt% of low-molecular-weight heparin. Because these tetrasaccharides are derived from heparin's antithrombin III-binding sites, we examined whether this method could be applied to estimate the anticoagulant activity of heparin. The content of 3-O-sulfo group-containing tetrasaccharides in a heparin correlated positively (r=0.8294) to heparin's anticoagulant activity.
摘要
用肝素酶2完全消化肝素可得到二糖和抗性四糖的混合物，这些抗性四糖在其还原端含有含3-O-磺基的葡糖胺残基。本文描述了对这些抗性四糖进行定量在线液相色谱-质谱分析的方法。用该方法分析了七种猪肠肝素和五种低分子量肝素的二糖和四糖组成。这些抗性四糖占肝素的5.3%至7.3wt%，占低分子量肝素的6.2%至8.3wt%。由于这些四糖源自肝素的抗凝血酶III结合位点，我们研究了该方法是否可用于估计肝素的抗凝活性。肝素中含3-O-磺基的四糖含量与肝素的抗凝活性呈正相关（r=0.8294）。
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