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Data for Assessing the detection limit of a minority solid-state form of a pharmaceutical by 1H double-quantum MAS NMR spectroscopy Keisuke Maruyoshi (2566843) Dinu Iuga (1345257) Abigail E. Watts (3801910) Colan E. Hughes (1296822) Kenneth D.M. Harris (1300911) Steven P. Brown (1296819) Drugs -- Testing Nuclear magnetic resonance spectroscopy Migrated from ePrints 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.<br><br>NMR experimental data set generated using Bruker TOPSPIN software, relating to figures 1 and 2. See README file for more information. 2017-08-03T00:00:00Z Dataset Dataset 10.82444/warw.33742561.v1 https://figshare.com/articles/dataset/Data_for_Assessing_the_detection_limit_of_a_minority_solid-state_form_of_a_pharmaceutical_by_1H_double-quantum_MAS_NMR_spectroscopy/33742561 CC BY 4.0