A cross-polarization magic-angle spinning 13C NMR characterization of the stable solid-state forms of cimetidine

Journal of Pharmaceutical Sciences
D A MiddletonD G Reid

Abstract

Proton decoupled, cross-polarization magic-angle spinning 13C NMR spectra of four polymorphic forms (A, B, C, and D) and a monohydrate form (M1) of the histamine H2 antagonist cimetidine were obtained, and the chemical shifts of the various forms were tabulated. A modified polarization inversion pulse sequence was used to distinguish quaternary, methine, methylene, and methyl carbon resonances and thereby assist spectral assignment. It is also shown that the solid-state form of cimetidine in a commercial formulation can be reliably ascertained by NMR, despite the presence in the spectrum of signals from organic excipients that are much more intense than those from the compound.

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Citations

Apr 28, 2001·Advanced Drug Delivery Reviews·D E Bugay
Sep 5, 2001·International Journal of Pharmaceutics·T WatanabeM Senna
Nov 14, 2002·International Journal of Pharmaceutics·Tomoyuki WatanabeMamoru Senna
Feb 11, 2014·Journal of Pharmaceutical and Biomedical Analysis·Natalia L CalvoTeodoro S Kaufman
Aug 9, 2003·Drug Development and Industrial Pharmacy·Nobuyuki SuzukiTakao Kawasaki
Feb 15, 2003·Journal of Pharmaceutical Sciences·Patrick A TishmackStephen R Byrn
Nov 23, 2015·The Journal of Chemical Physics·Keyton KalakewichJames K Harper
Jan 5, 2007·Physical Chemistry Chemical Physics : PCCP·Jillian Madine, David A Middleton
Feb 24, 2006·The Analyst·Robin K Harris
Aug 8, 2019·Nature Communications·Candelaria Guzmán-AfonsoYusuke Nishiyama
Apr 3, 2020·The Journal of Physical Chemistry. a·Sean T HolmesRobbie James Iuliucci
Jun 29, 1999·Analytical Chemistry·R K Gilpin, L A Pachla

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