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通过魔法角度旋转固态NMR探测Dabrafenib的同结构水合物和合物中的短距离相互作用

Sunil K Rai¹, Lokeswara Rao Potnuru¹, Nghia Tuan Duong²

¹Tata Institute of Fundamental Research Hyderabad, Hyderabad, Telangana 500046, India.

Analytical chemistry

|July 22, 2024

概括

这项研究使用固态NMR和计算方法来分析抗癌药物Dabrafenib的水合物和水合物形式. 它成功地量化了水和过氧化在晶体中的混合水,并揭示了溶剂相互作用.

科学领域:

固态化学固态化学
晶体学晶体学是指结晶学.
药物的配方药物的配方

背景情况:

达布拉费尼布 (DBF) 伪多态 (水合物 DBFH2O 和合物 DBFH2O2) 呈现同结构性质,但具有不同的热行为.
由于水和过氧化的共存,确定水在水晶中的固态度具有挑战性.

研究的目的:

为了描述溶剂分子对Dabrafenib伪多态分子局部环境的影响.
开发一种方法来量化水和过氧化混合在晶体空隙中的水分.
为了阐明水素过氧化物和Dabrafenib在晶格中的相互作用.

主要方法:

魔法角旋转 (MAS) 固态NMR (SSNMR) 谱学 (1H, 13C, 15N).
测量器包括投影机增强波 (GIPAW) 的计算.
1H-1H和1H-14N的NMR距离测量.
用于结构分析的X射线衍射和密度函数理论 (DFT).

主要成果:

SSNMR成功地分配了光谱峰值,并确定了同结构伪多重形之间的差异.
质子光谱测量了混合DBFH2O2形式的水与过氧化的比例.
核磁共振距离测量证实了3D分子包装,并阐明了H2O2-DBF相互作用和几何.

结论:

结合X射线衍射,量子化学计算和SSNMR的综合方法为研究结晶溶剂相互作用提供了实用的方法.
这种方法即使没有高分辨率的晶体结构或样本丰富,也有效.
这项研究提供了对Dabrafenib伪多态化合物的复杂溶剂安排的见解.

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