Pressure-assisted capillary electrophoresis-electrospray ion trap mass spectrometry for the analysis of heparin depolymerised disaccharides.
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.
Ruiz-Calero
V
V
Departament de Química Analítica, Facultat de Química, Universitat de Barcelona, Spain.
Moyano
E
E
Puignou
L
L
Galceran
M T
MT
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*
D004187:Disaccharides; D006493:Heparin