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19 F NMR Spectroscopy as a Highly Sensitive Method for the Direct Monitoring of Confined Crystallization within Nanoporous Materials
Author(s) -
Nartowski Karol P.,
Malhotra Diksha,
Hawarden Lucy E.,
Sibik Juraj,
Iuga Dinu,
Zeitler J. Axel,
Fábián László,
Khimyak Yaroslav Z.
Publication year - 2016
Publication title -
angewandte chemie
Language(s) - English
Resource type - Journals
eISSN - 1521-3757
pISSN - 0044-8249
DOI - 10.1002/ange.201602936
Subject(s) - crystallization , nanoporous , nuclear magnetic resonance spectroscopy , mesoporous material , magic angle spinning , nanoreactor , chemical engineering , spectroscopy , materials science , context (archaeology) , nanotechnology , chemistry , organic chemistry , catalysis , nanoparticle , paleontology , physics , quantum mechanics , engineering , biology
Abstract The introduction of fluorine into the structure of pharmaceuticals has been an effective strategy for tuning their pharmacodynamic properties, with more than 40 new drugs entering the market in the last 15 years. In this context, 19 F NMR spectroscopy can be viewed as a useful method for investigating the host–guest chemistry of pharmaceuticals in nanosized drug‐delivery systems. Although the interest in confined crystallization, nanosized devices, and porous catalysts is gradually increasing, understanding of the complex phase behavior of organic molecules confined within nanochambers or nanoreactors is still lacking. Using 19 F magic‐angle‐spinning NMR spectroscopy, we obtained detailed mechanistic insight into the crystallization of flufenamic acid (FFA) in a confined environment of mesoporous silica materials with different pore diameters (3.2–29 nm), providing direct experimental evidence for the formation of a molecular‐liquid‐like layer besides crystalline confined FFA form I.