Abstract
Many pharmaceutical samples have notably long 1H T1 (proton spin-lattice relaxation time), leading to lengthy experiments lasting several days in solid-state NMR studies. In this work, we propose the use of ball milling on the pharmaceutical samples to reduce the 1H T1, which also leads to enhanced sensitivity in {1H}-13C Cross-Polarization (CP) experiments due to reduced particle sizes and increased surface areas of the samples. Experimentally, we determined that depending on the substrates and milling time, the signal-to-noise ratio (S/N) of a 1D 13C CP spectrum can be increased by a factor of 3–6, which means that the experimental time can be shortened by a factor of 9–36. Furthermore, the application of simple ball-milling within a short time avoids the amorphization of the studied samples such that no signal due to amorphous state is observed in the 13C CP spectrum. This simple ball milling method used for sensitivity enhancement can be further applied in the SS-NMR studies of pharmaceutical samples.
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