Segregation analysis method for heparan disaccharide sulfate containing FlcNH3<+>

A technology of heparin sulfate and glucosamine, which is used in material separation, analysis materials, measuring devices, etc., can solve the problems of small content, difficult separation, and complicated processing, so as to improve the detection level and ensure the effect of drug safety.

Inactive Publication Date: 2015-09-16
FUZHOU UNIV
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Problems solved by technology

However, these methods are mainly used for the analysis of 8 heparan sulfate/heparan disaccharides containing GlcNAc residues and GlcNSO3 residues, while GlcNH3+ The content of heparan sulfate/heparan disaccharide residues in biological samples is small and difficult to separate, and there are few studies on qualitative and quantitative analysis and detection methods for them
Robert J. Linhardt et al. used the reacetylated isotope labeling m...

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  • Segregation analysis method for heparan disaccharide sulfate containing FlcNH3&lt;+&gt;
  • Segregation analysis method for heparan disaccharide sulfate containing FlcNH3&lt;+&gt;
  • Segregation analysis method for heparan disaccharide sulfate containing FlcNH3&lt;+&gt;

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Embodiment 1

[0047] This technical solution is used to analyze the disaccharide components of bovine kidney heparan sulfate biological samples, heparin sodium for commercially available drugs, and samples treated with high temperature and high pressure (121°C).

[0048] The separation and analysis method of heparan sulfate and heparin disaccharide containing N-non-substituted residues, the steps are as follows:

[0049] (1) Dissolve n-hexylamine in deionized water, adjust the pH value to 8.8 with formic acid, and prepare mobile phase A with a concentration of 30mM;

[0050] (2) Dissolve n-hexylamine in an acetonitrile solution with a volume percentage of 80%, adjust the pH value to 8.8 with formic acid, and prepare mobile phase B with a concentration of 30mM;

[0051] (3) Take 20 μg each of commercially available bovine kidney heparan sulfate, commercially available heparin sodium, and heparin sodium treated with high temperature and high pressure (121°C), and mix them with heparinase I, h...

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Abstract

The invention discloses a segregation analysis method for heparan disaccharide sulfate containing FlcNH3<+>. A mass spectrum peak area correcting factor can be used for the quantitative detection of herparan sulfate and herparan disaccharide in a practical biological sample. According to the method, heparan disaccharide sulfate containing FlcNH3<+> can be detected quickly, the content has an important effect of influence research on the anticoagulation effect of clinical drug (herparan) and the detection on the disaccharide component of a biological sample.

Description

technical field [0001] The invention belongs to the field of detection of medicines and raw materials, in particular to an N-non-substituted glucosamine-containing (GlcNH 3 + ) Separation and analysis method of heparan sulfate disaccharide. Background technique [0002] Heparin is a glycosaminoglycan drug with strong anticoagulant effect and is currently the drug of choice for the treatment of thromboembolic diseases. Heparan sulfate and heparin are composed of repeated disaccharide structural units linked by hexuronic acid and glucosamine with 1-4 glycosidic bonds, among which there are twelve representative disaccharide units, with N-acetylated Glucosamine (GlcNAc) residues, containing N-sulfated glucosamine (GlcNSO 3 ) residues of heparan sulfate / heparan disaccharides are the main form, while N-unsubstituted glucosamine (GlcNH 3 + ) residues of heparin disaccharides are relatively rare. The anticoagulant effect of heparin is related to a unique N-position highly sul...

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 魏峥林江慧肖晓毛杜家燕
Owner FUZHOU UNIV
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