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: 8168894
• 负责人: Parastoo Azadi
• 金额: $ 0.17万
• 依托单位: UNIVERSITY OF GEORGIA
• 依托单位国家: 美国
• 财政年份: 2010
• 资助国家: 美国
• 起止时间: 2010-04-10 至 2011-01-31
• 项目状态: 已结题
• 来源: https://reporter.nih.gov/project-details/8168894
• 关键词: Blood capillaries; Chemicals; Computer Retrieval of Information on Scientific Projects Database; Deuterium Oxide; Funding; Gases; Grant; Institution; Isotopes; Mass Spectrum Analysis; Measures; NMR Spectroscopy; NOESY; Protons; Pump; Relative (related person); Research; Research Personnel; Resources; Sampling; Scanning; Signal Transduction; Silicon Dioxide; Solutions; Solvents; Source; Spectrometry, Mass, Electrospray Ionization; Spectrum Analysis; Syringes; TOCSY; Temperature; Time; Tube; United States National Institutes of Health; Water; capillary; 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. 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 ¿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.

这个子项目是许多利用 由NIH/NCRR资助的中心赠款提供的资源。子项目和 研究者（PI）可能从另一个NIH来源获得了主要资金， 因此可以在其他CRISP条目中表示。列出的机构为 研究中心，而研究中心不一定是研究者所在的机构。 NMR光谱 将样品（30 mg）溶于氧化氘（99.9% D，Aldrich）中并冻干。 将样品溶解于96？L D2 O（99.96% D，剑桥同位素）中，加入4？L 50 mg/mL DSS，并将溶液置于3 mm Shigemi NMR管中。 一维质子、gCOSY、TOCSY、gHSQC、NOESY和gHMBC NMR光谱在Varian Inova-500光谱仪上在298 K（25 ℃）下获得。相对于内部DSS测量化学位移（H=0.000 ppm，C=0.000 ppm）。 进一步的实验细节可根据要求提供。 ESI质谱 在LCQ Advantage ESI-四极杆仪器上使用50%MeOH/水作为喷雾溶剂进行质谱分析。 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 <$C，鞘气流速为43，毛细管电压为-11.00 V，管透镜偏移为15.00 V。通过注射泵和石英毛细管以10 <$L/min输注约50 <$M溶液。在2 min扫描时间内进行信号平均。