(13)C Solid-state NMR chromatography by magic angle spinning (1)H T(1) relaxation ordered spectroscopy.
An efficient method to separate the (13)C NMR spectra of solid mixtures is introduced. The (1)H longitudinal (T(1)) relaxation time is used to separate the overlapping (13)C chemical shift spectra of solid mixtures via an inverse Laplace transform (ILT) of the relaxation dimension. The resulting 2D spectrum of the mixture contains separate (13)C spectra for each component of the mixture that are identical to (13)C spectra of the isolated materials. The separation is based on the equalization of (1)H T(1) values in a single domain by rapid (1)H spin diffusion and on the (1)H T(1) value differences between different domains. The introduction of a general ILT scheme enables efficient and reduced data acquisition time. The method is demonstrated on a mixture of two disaccharides and on a commercial drug containing several compounds.
Nishiyama
Yusuke
Y
JEOL Ltd., 3-1-2 Musashino, Akishima, Tokyo 196-8558, Japan. yunishiy@jeol.co.jp
Frey
Michael H
MH
Mukasa
Sseziwa
S
Utsumi
Hiroaki
H
D000082:Acetaminophen / Q000737:chemistry; D000409:Alanine / Q000737:chemistry; D000465:Algorithms; D002250:Carbon Radioisotopes / Q000737:chemistry*; D002475:Cellobiose / Q000737:chemistry; D003625:Data Collection; D003627:Data Interpretation, Statistical; D004574:Electromagnetic Fields; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D011522:Protons; D012015:Reference Standards; D012457:Salicylamides / Q000737:chemistry; D013395:Sucrose / Q000737:chemistry
D002250:Carbon Radioisotopes; D011522:Protons; D012457:Salicylamides; D002475:Cellobiose; D000082:Acetaminophen; D013395:Sucrose; C018935:ethenzamide; D000409:Alanine