Abstract
A capillary NMR flow probe was designed to generate high-resolution 1H NMR spectra at 600 MHz from the cleaved product of individual 160-μm Tentagel combinatorial chemistry beads. By injecting a dissolved sample sandwiched between an immiscible, perfluorinated organic liquid directly into the probe, NMR spectra of the product cleaved from single beads were acquired in just 1 h of spectrometer time without diffusional dilution. Sample handling efficiency on the single bead scale was comparable to that obtained with a bulk sample. Using the relative intensity of the DMSO-d5H versus the analyte signals in a fully relaxed CPMG spectrum, the amount of product cleaved from a single bead was determined to be 540 ± 170 pmol in one of the samples. Following the NMR data collection, the samples were examined with electrospray ionization mass spectrometry to provide additional structural information. By coupling with microliter-volume fluidic capabilities, the capillary flow probe described here will enable multidimensional characterization of single solid-phase resin products in an online manner.
Original language | English (US) |
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Pages (from-to) | 215-222 |
Number of pages | 8 |
Journal | Journal of Magnetic Resonance |
Volume | 153 |
Issue number | 2 |
DOIs | |
State | Published - 2001 |
Keywords
- Mass spectrometry
- Microcoil
- Nanoliter
- Nuclear magnetic resonance
- Tentagel beads
ASJC Scopus subject areas
- Molecular Biology
- Physical and Theoretical Chemistry
- Spectroscopy
- Radiology Nuclear Medicine and imaging
- Condensed Matter Physics