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Assessing the detection limit of a minority solid-state Form of a pharmaceutical by 1 H double-quantum magic-angle spinning nuclear magnetic resonance spectroscopy

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 1 H double-quantum magic-angle spinning nuclear magnetic resonance spectroscopy. Journal of Pharmaceutical Sciences 106 (11) , pp. 3372-3377. 10.1016/j.xphs.2017.07.014

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Abstract

The lower detection limit for 2 distinct crystalline phases by 1H magic-angle spinning (MAS) solid-state nuclear magnetic resonance (NMR) is investigated for a minority amount of cimetidine (anhydrous polymorph A) in a physical mixture with the anhydrous HCl salt of cimetidine. Specifically, 2-dimensional 1H double-quantum (DQ) MAS NMR spectra of polymorph A and the anhydrous HCl 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 HCl salt is a concentration of 1% w/w.

Item Type: Article
Date Type: Publication
Status: Published
Schools: Chemistry
Publisher: WileyBlackwell
ISSN: 0022-3549
Date of First Compliant Deposit: 31 August 2017
Date of Acceptance: 18 July 2017
Last Modified: 12 Nov 2017 00:31
URI: http://orca.cf.ac.uk/id/eprint/104177

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