کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
10162535 1114333 2013 12 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Solid-State NMR Analysis of a Boron-Containing Pharmaceutical Hydrochloride Salt
موضوعات مرتبط
علوم پزشکی و سلامت داروسازی، سم شناسی و علوم دارویی اکتشاف دارویی
پیش نمایش صفحه اول مقاله
Solid-State NMR Analysis of a Boron-Containing Pharmaceutical Hydrochloride Salt
چکیده انگلیسی
A novel crystalline form of the boron-containing antibacterial drug (S)-3-(aminomethyl)-7-(3-hydroxypropoxy)benzo[c][1,2]oxaborol-1(3H)-ol hydrochloride is studied by solid-state nuclear magnetic resonance (SSNMR) and single-crystal X-ray diffraction techniques. After determination of the crystal structure by X-ray diffraction, SSNMR spectroscopy of this form is performed to obtain structural information using experimental approaches based on dipolar correlation, chemical shift analysis, and quadrupolar interaction analysis.1H SSNMR experiments at 16.4 T using magic-angle spinning (MAS) and homonuclear dipolar decoupling, 2D SSNMR experiments based on1H-13C and1H-11B dipolar heteronuclear correlation, and density functional theory (DFT) calculations are combined in a novel approach to obtain a nearly complete assignment of the1H spectrum of this crystalline phase.11B and35Cl chemical shift and quadrupolar parameters are obtained using the analysis of MAS spectra and are found to be accurately reproduced using DFT calculations. NMR chemical shielding and electric field gradient parameters obtained using these methods are related to hydrogen-bonding trends in the crystal structure. The results illustrate the increasing capability of SSNMR techniques involving1H,11B, and35Cl SSNMR in the analysis of the crystal structure of a pharmaceutical compound containing covalently bonded boron. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:3705-3716, 2013
ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Pharmaceutical Sciences - Volume 102, Issue 10, October 2013, Pages 3705-3716
نویسندگان
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