Reduction of the 13C cross-polarization experimental time for pharmaceutical samples with long T1 by ball milling in solid-state NMR
作者： Xiaobing Lou , Ming Shen , Chao Li , Qun Chen , Bingwen Hu
DOI: 10.1016/J.SSNMR.2018.08.001
关键词: Proton 、 Materials science 、 Reduction (complexity) 、 Analytical chemistry 、 Solid-state nuclear magnetic resonance 、 Ball mill 、 Work (thermodynamics) 、 Sensitivity (control systems) 、 Amorphous solid 、 Particle
摘要: 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 reduce T1, which also leads enhanced sensitivity {1H}-13C Cross-Polarization (CP) due reduced particle sizes and increased surface areas samples. Experimentally, determined that depending substrates time, signal-to-noise ratio (S/N) a 1D 13C CP spectrum can be by factor 3-6, means experimental time shortened 9-36. Furthermore, application simple ball-milling within short avoids amorphization studied such no signal amorphous state is observed spectrum. This method used for enhancement further applied SS-NMR studies
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