1H NMR Characterization of the Product from Single Solid-Phase Resin Beads Using Capillary NMR Flow Probes
✍ Scribed by Michael E. Lacey; Jonathan V. Sweedler; Cynthia K. Larive; Adrian J. Pipe; R.Duncan Farrant
- Publisher
- Elsevier Science
- Year
- 2001
- Tongue
- English
- Weight
- 134 KB
- Volume
- 153
- Category
- Article
- ISSN
- 1090-7807
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✦ Synopsis
A capillary NMR flow probe was designed to generate highresolution 1 H 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-d 5 H 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.