title: Pressure-assisted capillary electrophoresis-electrospray ion trap mass spectrometry for the analysis of heparin depolymerised disaccharides.
abstract: A pressure-assisted capillary electrophoresis-ion trap mass spectrometry method was developed for the analysis of eight heparin-derived disaccharides. A 30 mM formic acid buffer at pH 3.20 was selected as running electrolyte, and the separation was performed by the simultaneous application of a CE voltage of -30 kV and an overimposed pressure of 0.5 p.s.i. (3.45 kPa). The application of pressure assistance was needed to provide stable electrospray conditions for successful coupling. The linearity of the CE-MS and CE-MS-MS methods was checked under these conditions. Quality parameters such as run-to-run precision and limits of detection were established in both CE-MS and CE-MS-MS modes. Finally, enzymatically depolymerised bovine and porcine mucosal heparins were analysed in this CE-MS system and the characteristic relative molar percentages of major and minor disaccharides were calculated.
authors.affiliation: Departament de Química Analítica, Facultat de Química, Universitat de Barcelona, Spain.
authors.forename: V
authors.initials: V
authors.lastname: Ruiz-Calero
authors.forename: E
authors.initials: E
authors.lastname: Moyano
authors.forename: L
authors.initials: L
authors.lastname: Puignou
authors.forename: M T
authors.initials: MT
authors.lastname: Galceran
mesh_terms: D004187:Disaccharides / Q000032:analysis* / Q000737:chemistry; D019075:Electrophoresis, Capillary / Q000379:methods*; D006493:Heparin / Q000737:chemistry*; D011312:Pressure; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
chemical_list: D004187:Disaccharides; D006493:Heparin