New Techniques for Solid-State NMR Studies of Pharmaceuticals

堪萨斯大学的Eric J. Munson教授得到了分析和表面化学项目的支持，以开发使用固态NMR光谱（SSNMR）改进药物分析的方法。 一个魔角旋转（MAS）核磁共振探针，包含多个旋转系统正在建设中。 探头设计使旋转系统能够快速进出静磁场的均匀区域。 在获取一个样品的光谱的同时，其他样品的磁化在磁场的不均匀区域中恢复平衡。 与传统MAS探针相比，多样品能力提高了灵敏度和通量。 该项目还在调查与新药物化合物配方有关的基本问题。 一个领域集中于提高固态NMR光谱的能力，以识别、检测和定量药物固体的多晶型物、溶剂化物和无定形形式。 另一个是确定弛豫和线宽如何与药物的物理化学性质相关，如粒度和晶体缺陷。 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技术为药物制剂的表征提供了新的工具。 这些进展也可以广泛应用于药物和样品的分析，包括玻璃，聚合物和催化剂。 该项目正在为研究生提供培训，并促进与制药业的合作。

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.