Chromatography-mass spectrometry detection method for electrophoresis hydrophilic interaction of sulodexide

Abstract

The invention provides a chromatography-mass spectrometry detection method for electrophoresis hydrophilic interaction of sulodexide and belongs to the technical field of detection of medicines, crudedrugs and raw materials. According to the method provided by the invention, the difference of electrophoretic mobility of each component in the sulodexide is utilized and the components are separatedthrough agarose gel electrophoresis; then the components are extracted by utilizing an ion exchange centrifugal column; then each component is enzymolyzed into a composition unit by utilizing the specificity of an enzyme; finally, each component of the sulodexide is detected through a chromatography-mass spectrometry method for the hydrophobic interaction, so that qualitative and relatively quantitative analysis is carried out on rapid mobile heparin (FMH), slow mobile heparin (SMH) and dermatan sulfate (DS) of the sulodexide, and a fine structure and a terminal structure of each component are identified and analyzed.

Description

technical field [0001] The invention relates to an electrophoretic hydrophilic interaction chromatography-mass spectrometry detection method for sulodexide, in particular to a method for separating sulodexide by electrophoresis, and then using ion-exchange spin columns and enzymes to extract and degrade the drug , and finally a method for qualitative and relative quantitative analysis of the structure through hydrophilic interaction chromatography and mass spectrometry, belonging to the technical field of medicine, raw material medicine and raw material detection. Background technique [0002] Sulodexide is extracted and refined from pig small intestinal mucosa, and is an antithrombotic drug used clinically to treat various cardiovascular diseases. Sulodexide has multiple biological functions such as anticoagulant, antithrombotic, anti-cardiovascular disease and hypolipidemic. Compared with heparin, an anticoagulant drug commonly used in clinical practice, sulodexide has st...

AI Technical Summary

Problems solved by technology

Unlike heparin, an anticoagulant drug commonly used in clinical practice, sulodexide is mainly composed of two different glycosaminoglycans, including fast moving heparin (FMH) with a natural mixture content of about 80% and sulfuric acid with a content of about 20% Dermatin (DS) composition, in addition, the presence of slow-moving heparin (SMH) at a content of no more than 2%, which also makes the analysis of sulodexide very difficult

[0003] Using common analytical methods to analyze sulodexide, gel permeation chromatography (GPC) can only divide sulodexide into two components, heparan sulfate (HS) and dermatan sulfate (DS), and cannot achieve a complete baseline Separation; nuclear magnetic resonance spectroscopy (NMR) can provide compositional information, including structural features and monosaccharide substitutions, but cannot provide more fine structure information; due to the large molecular weight and high heterogeneity of HS and DS, it is difficult to use chromatography-mass spectrometry (LC-MS) analysis, the chromatographic separation

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