Pressure-assisted capillary electrophoresis-electrospray ion trap mass spectrometry for the analysis of heparin depolymerised disaccharides |
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Authors: | Ruiz-Calero V Moyano E Puignou L Galceran M T |
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Affiliation: | Departament de Química Analítica, Facultat de Química, Universitat de Barcelona, Spain. |
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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. |
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