New Techniques for Solid-State NMR Studies of Pharmaceuticals

药物固态核磁共振研究新技术

• 批准号: 0416214
• 负责人: Eric Munson
• 金额: --
• 依托单位: University of Kansas Center for Research Inc
• 依托单位国家: 美国
• 项目类别: Standard Grant
• 财政年份: 2004
• 资助国家: 美国
• 起止时间: 2004-08-01 至 2007-07-31
• 项目状态: 已结题
• 来源: https://www.nsf.gov/awardsearch/showAward?AWD_ID=0416214&HistoricalAwards=false
• 关键词: New; Techniques; Solid; State; NMR

Professor Eric J. Munson of the University of Kansas is supported by the Analytical and Surface Chemistry program to develop methods to improve the analysis of pharmaceuticals using solid-state NMR spectroscopy (SSNMR). A magic-angle spinning (MAS) NMR probe that contains multiple spinning systems is being constructed. The probe design enables the spinning systems to be rapidly shuttled in and out of the homogeneous region of the static magnetic field. While the spectrum of one sample is being acquired, the magnetization of the other samples are returning to equilibrium in the inhomogeneous region of the field. The multiple sample capabilities increase sensitivity and throughput compared to conventional MAS probes. The project is also investigating fundamental problems related to the formulation of new drug compounds. One area focuses on improving the capabilities of solid-state NMR spectroscopy to identify, detect, and quantify polymorphs, solvates, and amorphous forms of a pharmaceutical solid. Another is determining how relaxation and line width are related to the physicochemical properties of the drug, such as particle size and crystal defects. A third area is applying the knowledge gained from measured NMR parameters to drug stability, with the ultimate goal of using solid-state NMR as a predictive tool for early identification of stable formulations.The SSNMR technology being developed is providing new tools for the characterization of drug formulations. The advances can also be applied broadly to the analysis of pharmaceuticals and samples that include glasses, polymers, and catalysts. The project is providing training for graduate students and enabling collaborations with the pharmaceutical industry.

堪萨斯大学的 Eric J. Munson 教授在分析和表面化学项目的支持下，开发了使用固态核磁共振波谱 (SSNMR) 改进药物分析的方法。 包含多个旋转系统的魔角旋转（MAS）核磁共振探头正在建造中。 探头设计使旋转系统能够快速进出静磁场的均匀区域。 当采集一个样品的光谱时，其他样品的磁化强度在场的不均匀区域中恢复平衡。 与传统 MAS 探针相比，多样品功能提高了灵敏度和通量。 该项目还在研究与新药化合物配方相关的基本问题。 其中一个领域专注于提高固态核磁共振波谱识别、检测和量化药物固体的多晶型物、溶剂化物和无定形形式的能力。 另一个是确定弛豫和线宽与药物的物理化学性质（例如粒径和晶体缺陷）之间的关系。 第三个领域是将从测量的 NMR 参数中获得的知识应用于药物稳定性，最终目标是使用固态 NMR 作为早期鉴定稳定制剂的预测工具。正在开发的 SSNMR 技术正在为表征药物稳定性提供新工具。药物制剂。 这些进步还可广泛应用于药物和样品（包括玻璃、聚合物和催化剂）的分析。 该项目为研究生提供培训，并促进与制药行业的合作。