A new generation of microscale, nuclear magnetic resonance (CapNMR) probe technology employs two independent detection elements to accommodate two samples simultaneously. Each detection element in the dual-sample CapNMR probe (DSP) delivers the same spectral resolution and S/N as in a CapNMR probe configured to accommodate one sample at a time. A high degree of electrical isolation allows the DSP to be used in a variety of data acquisition modes. Both samples are shimmed simultaneously to achieve high spectral resolution for simultaneous data acquisition, or alternatively, a flowcell-specific shim set is readily called via spectrometer subroutines to enable acquisition from one sample while the other is being loaded. An automation system accommodates loading of two samples via dual injection ports on an autosampler and two completely independent flowpaths leading to dedicated flowcells in the DSP probe.
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http://dx.doi.org/10.1021/ac101003f | DOI Listing |
Cells
November 2022
Institute of Pharmacy/Pharmacognosy, CCB-Centrum of Chemistry and Biomedicine, University of Innsbruck, Innrain 80-82, A-6020 Innsbruck, Austria.
Gaining structural information is a must to allow the unequivocal structural characterization of analytes from natural sources. In liquid state, NMR spectroscopy is almost the only possible alternative to HPLC-MS and hyphenating the effluent of an analyte separation device to the probe head of an NMR spectrometer has therefore been pursued for more than three decades. The purpose of this review article was to demonstrate that, while it is possible to use mass spectrometry and similar methods to differentiate, group, and often assign the differentiating variables to entities that can be recognized as single molecules, the structural characterization of these putative biomarkers usually requires the use of NMR spectroscopy.
View Article and Find Full Text PDFAnal Chem
September 2010
Protasis/MRM Corporation, 101 West Tomaras Avenue, Savoy, Illinois 61874, USA.
A new generation of microscale, nuclear magnetic resonance (CapNMR) probe technology employs two independent detection elements to accommodate two samples simultaneously. Each detection element in the dual-sample CapNMR probe (DSP) delivers the same spectral resolution and S/N as in a CapNMR probe configured to accommodate one sample at a time. A high degree of electrical isolation allows the DSP to be used in a variety of data acquisition modes.
View Article and Find Full Text PDFAnal Bioanal Chem
August 2007
Department of Chemistry, University of California, Riverside, CA 92521, USA.
The isolation and purification of sufficient quantities of heparin-derived oligosaccharides for characterization by NMR is a tedious and time-consuming process. In addition, the structural complexity and microheterogeneity of heparin makes its characterization a challenging task. The improved mass-sensitivity of microcoil NMR probe technology makes this technique well suited for characterization of mass-limited heparin-derived oligosaccharides.
View Article and Find Full Text PDFAnal Chem
January 2007
Department of Medicinal Chemistry, The Danish University of Pharmaceutical Sciences, Universitetsparken 2, DK-2100 Copenhagen, Denmark.
Two major development areas in HPLC-NMR hyphenation are postcolumn solid-phase extraction (HPLC-SPE-NMR) and capillary separations with NMR detection by means of solenoidal microcoils (CapNMR). These two techniques were combined off-line into HPLC-SPE-CapNMR, which combines the advantage of high loadability of normal-bore HPLC columns with high mass sensitivity of capillary NMR probes with an active volume of 1.5 microL.
View Article and Find Full Text PDFAngew Chem Int Ed Engl
November 2006
Biological Chemistry and Molecular Pharmacology, Harvard Medical School, 250 Longwood Avenue, Boston, MA 02115, USA.
Capillary NMR (CapNMR) spectroscopy has emerged as a major breakthrough for increasing the mass-sensitivity of NMR spectroscopic analysis and enabling the combination of NMR spectroscopy with other analytical techniques. Not only is the acquisition of high-sensitivity spectra getting easier but the quality of CapNMR spectra obtained in many small-molecule applications exceeds what can be accomplished with conventional designs. This Minireview discusses current CapNMR technology and its applications for the characterization of mass-limited, small-molecule and protein samples, the rapid screening of small-molecule or protein libraries, as well as hyphenated techniques that combine CapNMR with other analytical methods.
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