Multiple-sample probe for solid-state NMR studies of pharmaceuticals.
Solid-state NMR spectroscopy (SSNMR) is an extremely powerful technique for the analysis of pharmaceutical dosage forms. A major limitation of SSNMR is the number of samples that can be analyzed in a given period of time. A solid-state magic-angle spinning (MAS) probe that can simultaneously acquire up to seven SSNMR spectra is being developed to increase throughput/signal-to-noise ratios. A prototype probe incorporating two MAS modules has been developed and spectra of ibuprofen and aspirin have been acquired simultaneously. This version is limited to being a two-module probe due to large amounts of space required for the tuning elements located next to the MAS modules. A new probe design incorporating coaxial transmission lines and smaller MAS modules has been constructed. This probe allows for close proximity of the MAS modules (within 3 cm), adequate proton decoupling power (>50 kHz), and the capability of remote tuning and sample changing. Spectra of hexamethylbenzene (HMB) have been acquired and show signal-to-noise ratios comparable to existing SSNMR probes. Adamantane line widths are also comparable to conventional probe technology. Decoupling powers of 70 kHz have been achieved using a MAS module suitable for 3 cm spacing between modules. Remote tuning has also been achieved with this new coaxial transmission line design. This probe design can be easily scaled to incorporate multiple MAS modules, which is a limitation of the previous design. The number of modules that can be incorporated is only limited by the number of transmission lines that will fit in a cross-sectional diameter of the bore and the axial field length of the magnet.
Nelson
Benjamin N
BN
Department of Pharmaceutical Chemistry, University of Kansas, 2095 Constant Avenue, Lawrence, KS 66047, USA.
Schieber
Loren J
LJ
Barich
Dewey H
DH
Lubach
Joseph W
JW
Offerdahl
Thomas J
TJ
Lewis
David H
DH
Heinrich
John P
JP
Munson
Eric J
EJ
D045424:Complex Mixtures / Q000032:analysis* / Q000737:chemistry; D004867:Equipment Design; D019544:Equipment Failure Analysis; D009682:Magnetic Resonance Spectroscopy / Q000295:instrumentation* / Q000379:methods*; D015336:Molecular Probe Techniques / Q000295:instrumentation*; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014159:Transducers
D045424:Complex Mixtures; D004364:Pharmaceutical Preparations