GLYCOSYL COMPOSITION ANALYSIS OF PORCINE INTESTINAL HEPARINS

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1H-NMR analysis was performed on a Varian Inova 600-MHz spectrometer. The sample was deuterium-exchanged by lyophilization from D2O and dissolved in 0.5 mL DMSO-d6/D2O 982. The 1D 1H-NMR spectrum was obtained at 308(K (35(C) at 600 MHz using presaturation of the residual HOD signal. Chemical shifts were measured relative to the residual protonated DMSO-d6 at 2.503 ppm (measured indirectly relative to TMS=0.0ppm). The positive ion mode FAB mass spectrum was obtained using the first two sectors of a JEOL SX/SX102A tandem four-sector mass spectrometer operated at an acceleration potential of 10 kV. Linear upward scanning was employed such that the mass range from m/z 100 to 2500 is scanned in 1 minute. Application of both techniques confirmed the identity of the ganglioside with respect to the structure of the glycan, the molecular weight distribution and type of ceramides present, and the overall purity.