快速 F 魔角旋转核磁共振用于 blockbuster 药物中活性药物成分的结构表征。
Fast F Magic-Angle Spinning Nuclear Magnetic Resonance for the Structural Characterization of Active Pharmaceutical Ingredients in Blockbuster Drugs.
机构信息
Department of Chemistry and Biochemistry, University of Delaware, Newark, Delaware 19716, United States.
Pittsburgh Center for HIV Protein Interactions, University of Pittsburgh School of Medicine, 1051 Biomedical Science Tower 3, 3501 Fifth Avenue, Pittsburgh, Pennsylvania 15261, United States.
出版信息
Anal Chem. 2021 Sep 28;93(38):13029-13037. doi: 10.1021/acs.analchem.1c02917. Epub 2021 Sep 13.
Abstract
Fluorinated drugs occupy a large and growing share of the pharmaceutical market. Here, we explore high-frequency, 60 to 111 kHz, F magic-angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy for the structural characterization of fluorinated active pharmaceutical ingredients in commercial formulations of seven blockbuster drugs: Celebrex, Cipro, Crestor, Levaquin, Lipitor, Prozac, and Zyvox. F signals can be observed in a single scan, and spectra with high signal-to-noise ratios can be acquired in minutes. F spectral parameters, such as chemical shifts and line widths, are sensitive to both the nature of the fluorine moiety and the formulation. We anticipate that the fast F MAS NMR-based approach presented here will be valuable for the rapid analysis of fluorine-containing drugs in a wide variety of formulations.
摘要
含氟药物占据了医药市场的很大一部分并且其市场份额还在不断增长。在这里，我们探索了高频（60 到 111 千赫兹）氟魔角旋转（MAS）核磁共振（NMR）光谱技术，该技术用于对七种重磅炸弹药物（塞来昔布、环丙沙星、立普妥、左氧氟沙星、阿立哌唑、左洛复和利奈唑胺）的商业配方中的含氟活性药物成分进行结构特征描述。氟信号可以在单次扫描中观察到，并且可以在几分钟内获得具有高信噪比的光谱。氟光谱参数，如化学位移和谱线宽度，对氟原子部分的性质和制剂都很敏感。我们预计，这里提出的快速基于氟 MAS NMR 的方法将有助于快速分析各种制剂中的含氟药物。
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