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Assessing the detection limit of a minority solid-state form of a pharmaceutical by 1H double-quantum MAS NMR spectroscopy
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Maruyoshi, Keisuke, Iuga, Dinu, Watts, Abigail E., Hughes, Colan E., Harris, Kenneth D. M. and Brown, Steven P. (2017) Assessing the detection limit of a minority solid-state form of a pharmaceutical by 1H double-quantum MAS NMR spectroscopy. Journal of Pharmaceutical Sciences, 106 (11). pp. 3372-3377. doi:10.1016/j.xphs.2017.07.014 ISSN 0022-3549.
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Official URL: http://dx.doi.org/10.1016/j.xphs.2017.07.014
Abstract
The lower detection limit for two distinct crystalline phases by 1H magic-angle spinning (MAS) solid-state NMR is investigated for a minority amount of cimetidine (anhydrous polymorph A) in a physical mixture with the anhydrous hydrochloride salt of cimetidine. Specifically, two-dimensional 1H double-quantum (DQ) MAS spectra of polymorph A and the anhydrous hydrochloride salt constitute fingerprints for the presence of each of these solid forms. For solid-state NMR data recorded at a 1H Larmor frequency of 850 MHz and a MAS frequency of 30 kHz on ~10 mg of sample, it is shown that, by following the pair of cross peaks at a 1H DQ frequency of 7.4 + 11.6 = 19.0 ppm that are unique to polymorph A, the level of detection for polymorph A in a physical mixture with the anhydrous hydrochloride salt is a concentration of 1% w/w.
Item Type: | Journal Article | |||||||||||||||||||||
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Subjects: | Q Science > QD Chemistry R Medicine > RM Therapeutics. Pharmacology |
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Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | |||||||||||||||||||||
Library of Congress Subject Headings (LCSH): | Drugs -- Testing, Nuclear magnetic resonance spectroscopy | |||||||||||||||||||||
Journal or Publication Title: | Journal of Pharmaceutical Sciences | |||||||||||||||||||||
Publisher: | John Wiley & Sons, Inc. | |||||||||||||||||||||
ISSN: | 0022-3549 | |||||||||||||||||||||
Official Date: | November 2017 | |||||||||||||||||||||
Dates: |
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Volume: | 106 | |||||||||||||||||||||
Number: | 11 | |||||||||||||||||||||
Page Range: | pp. 3372-3377 | |||||||||||||||||||||
DOI: | 10.1016/j.xphs.2017.07.014 | |||||||||||||||||||||
Status: | Peer Reviewed | |||||||||||||||||||||
Publication Status: | Published | |||||||||||||||||||||
Access rights to Published version: | Open Access (Creative Commons) | |||||||||||||||||||||
Date of first compliant deposit: | 1 August 2017 | |||||||||||||||||||||
Date of first compliant Open Access: | 1 August 2017 | |||||||||||||||||||||
RIOXX Funder/Project Grant: |
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