Data for Assessing the detection limit of a minority solid-state form of a pharmaceutical by 1H double-quantum MAS NMR spectroscopy

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.