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.

该子项目是利用资源的众多研究子项目之一 由 NIH/NCRR 资助的中心拨款提供 该子项目的主要支持。 并且子项目的主要研究者可能是由其他来源提供的， 包括其他 NIH 来源的子项目可能列出的总成本。 代表子项目使用的中心基础设施的估计数量， NCRR 赠款不直接向子项目或子项目工作人员提供资金。 方法： 核磁共振波谱 将样品（30 mg）溶解在氧化氘（99.9% D，Aldrich）中并冻干。将样品溶解在 96 ¿ L D2O（99.96 % D，剑桥同位素），4 ¿添加 L 50 mg/mL DSS，并将溶液置于 3-mm Shigemi NMR 管中，在 Varian Inova-500 光谱仪上于 298 下采集 gCOSY、TOCSY、gHSQC、NOESY 和 gHMBC NMR 谱。 K (25 °C) 相对于内部 DSS 测量化学位移 (¿H=0.000 ppm， ¿C=0.000 ppm）可根据要求提供更多实验细节。 电喷雾质谱仪 使用 50% MeOH/水作为喷雾溶剂在 LCQ Advantage ESI 四极杆仪器上进行质谱分析，该仪器在三硫酸化肝素二糖 I-S 上调谐，喷雾电压为 3.80 kV，毛细管温度为 200 ¿ C，鞘气流速 43，毛细管电压 -11.00 V，管透镜偏移 15.00 V。A ~50 ¿ M溶液通过注射泵和二氧化硅毛细管在10 ¿ L/min 在 2 分钟扫描时间内进行信号平均。