NMR SPECTROSCOPY AND MASS SPECTROMETRY OF 2 SAMPLES

University Of Georgia, Athens GA

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Abstract

This subproject is one of many research subprojects utilizing the resources provided by a Center grant funded by NIH/NCRR. The subproject and investigator (PI) may have received primary funding from another NIH source, and thus could be represented in other CRISP entries. The institution listed is for the Center, which is not necessarily the institution for the investigator. NMR Spectroscopy The sample (30 mg) was dissolved in deuterium oxide (99.9 % D, Aldrich) and lyophilized. The sample was dissolved in 96 [unreadable]L D2O (99.96 % D, Cambridge Isotope), 4 [unreadable]L 50 mg/mL DSS was added, and the solution placed in a 3-mm Shigemi NMR tube. 1-D Proton, gCOSY, TOCSY, gHSQC, NOESY, and gHMBC NMR spectra were acquired on a Varian Inova-500 spectrometer at 298 K (25 [unreadable]C). Chemical shifts were measured relative to internal DSS ([unreadable]H=0.000 ppm, [unreadable]C=0.000 ppm). Further experimental details are available upon request. ESI Mass Spectrometry Mass spectrometry was performed on an LCQ Advantage ESI-quadrupole instrument using 50% MeOH/water as spray solvent. The instrument was tuned on the trisulfated heparin disaccharide I-S. Spray voltage was 3.80 kV, capillary temperature 200 [unreadable]C, sheath gas flow rate 43, capillary voltage -11.00 V, and tube lens offset 15.00 V. A ~50 [unreadable]M solution was infused via syringe pump and silica capillary at 10 [unreadable]L/min. Signal averaging was performed over 2 min scan time.