NMR SPECTROSCOPY AND MASS SPECTROMETRY OF 2 SAMPLES

2 个样品的核磁共振波谱和质谱分析

• 批准号: 8361827
• 负责人: Parastoo Azadi
• 金额: $ 0.18万
• 依托单位: UNIVERSITY OF GEORGIA
• 依托单位国家: 美国
• 财政年份: 2011
• 资助国家: 美国
• 起止时间: 2011-02-01 至 2012-01-31
• 项目状态: 已结题
• 来源: https://reporter.nih.gov/project-details/8361827
• 关键词: Blood capillaries; Chemicals; Deuterium Oxide; Funding; Gases; Grant; Isotopes; Mass Spectrum Analysis; Measures; Methods; NMR Spectroscopy; NOESY; National Center for Research Resources; Principal Investigator; Protons; Pump; Relative (related person); Research; Research Infrastructure; Resources; Sampling; Scanning; Signal Transduction; Silicon Dioxide; Solutions; Solvents; Source; Spectrometry, Mass, Electrospray Ionization; Syringes; TOCSY; Temperature; Time; Tube; United States National Institutes of Health; Water; capillary; cost; heparin disaccharide; instrument; lens; voltage

This subproject is one of many research subprojects utilizing the resources provided by a Center grant funded by NIH/NCRR. Primary support for the subproject and the subproject's principal investigator may have been provided by other sources, including other NIH sources. The Total Cost listed for the subproject likely represents the estimated amount of Center infrastructure utilized by the subproject, not direct funding provided by the NCRR grant to the subproject or subproject staff. Methods: NMR Spectroscopy The sample (30 mg) was dissolved in deuterium oxide (99.9 % D, Aldrich) and lyophilized. The sample was dissolved in 96 ¿L D2O (99.96 % D, Cambridge Isotope), 4 ¿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 ¿C). Chemical shifts were measured relative to internal DSS (¿H=0.000 ppm, ¿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 ¿C, sheath gas flow rate 43, capillary voltage -11.00 V, and tube lens offset 15.00 V. A ~50 ¿M solution was infused via syringe pump and silica capillary at 10 ¿L/min. Signal averaging was performed over 2 min scan time.

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