“…21,[42][43][44][45][46] The introduction of an inverse-detection microprobe designed for 3-mm diameter tubes with total sample volumes of ∼140 µL and observe volumes of ∼60 µL added further capabilities to small-volume NMR. [47][48][49][50][51] By reducing the sample size to a 1.7-mm diameter tube, rapid data acquisition on reduced sample amounts was enabled for inverse-detection microprobes. [52][53][54]…”
Section: B Reduction In Saddle-type Coil Sizementioning
confidence: 99%
“…Virtually all commercial NMR probe manufacturers now offer probes which utilize the increased sensitivity of small saddle coils. The first significant development involved Varian's use of 1.7-mm tubes for both 1 H and 13 C NMR of mass-limited samples. ,− The introduction of an inverse-detection microprobe designed for 3-mm diameter tubes with total sample volumes of ∼140 μL and observe volumes of ∼60 μL added further capabilities to small-volume NMR. − By reducing the sample size to a 1.7-mm diameter tube, rapid data acquisition on reduced sample amounts was enabled for inverse-detection microprobes. − 1 Examples of two RF coil geometries: (A) saddle type, (B) solenoid.…”
Section: B Reduction In Saddle-type Coil Sizementioning
Dean L. Olson (first row, right) completed his Ph.D. degree in Analytical Chemistry from the University of Illinois in 1994. He then joined the academic research group of Professor Sweedler performing the first high-resolution and sensitivity studies with nanoliter-volume NMR microcoils. He also conducted the first experiments using high-resolution NMR as a detector for capillary electrophoresis. He is now employed at MRM Corp. (Savoy, IL) conducting research toward the commercial development and application of capillarybased NMR probes. Andrew G. Webb (second row, right) received his Ph.D. degree in Medicinal Chemistry from the University of Cambridge in 1990 under Professor Laurie Hall. He was a postdoctoral researcher in the Department of Radiology at the University of Florida before joining the faculty in the Department of Electrical and Computer Engineering at the University of Illinois at Urbana−Champaign.He is currently an Associate Professor, with a full appointment in The Beckman Institute for Advanced Science and Technology. His research areas include the design of microcoils for NMR of mass-limited samples, the use of MRI temperature mapping for hyperthermia, and human brain mapping using functional MRI. Jonathan V. Sweedler (second row, left) received his Ph.D. degree in Analytical Chemistry from the University of Arizona in 1989 under Professor M. Bonner Denton and then spent 3 years at Stanford with Professors Richard Zare and Richard Scheller developing new methods to study neurotransmitters in individual neurons. He is currently a Professor of Chemistry, Neuroscience, and of the Beckman Institute for Advanced Science and Technology at the University of Illinois. His current research interests are twofold: first, he is developing information-rich methods with improved mass sensitivity for nanoliter-volume samples, including microcoil NMR, mass spectrometric imaging, and capillary-scale separations. In addition, he applies these techniques to understanding the role of neurotransmitter and neuropeptide co-transmission and the regulation of behavior in well-defined neuronal networks of opisthobranch molluscs.
“…21,[42][43][44][45][46] The introduction of an inverse-detection microprobe designed for 3-mm diameter tubes with total sample volumes of ∼140 µL and observe volumes of ∼60 µL added further capabilities to small-volume NMR. [47][48][49][50][51] By reducing the sample size to a 1.7-mm diameter tube, rapid data acquisition on reduced sample amounts was enabled for inverse-detection microprobes. [52][53][54]…”
Section: B Reduction In Saddle-type Coil Sizementioning
confidence: 99%
“…Virtually all commercial NMR probe manufacturers now offer probes which utilize the increased sensitivity of small saddle coils. The first significant development involved Varian's use of 1.7-mm tubes for both 1 H and 13 C NMR of mass-limited samples. ,− The introduction of an inverse-detection microprobe designed for 3-mm diameter tubes with total sample volumes of ∼140 μL and observe volumes of ∼60 μL added further capabilities to small-volume NMR. − By reducing the sample size to a 1.7-mm diameter tube, rapid data acquisition on reduced sample amounts was enabled for inverse-detection microprobes. − 1 Examples of two RF coil geometries: (A) saddle type, (B) solenoid.…”
Section: B Reduction In Saddle-type Coil Sizementioning
Dean L. Olson (first row, right) completed his Ph.D. degree in Analytical Chemistry from the University of Illinois in 1994. He then joined the academic research group of Professor Sweedler performing the first high-resolution and sensitivity studies with nanoliter-volume NMR microcoils. He also conducted the first experiments using high-resolution NMR as a detector for capillary electrophoresis. He is now employed at MRM Corp. (Savoy, IL) conducting research toward the commercial development and application of capillarybased NMR probes. Andrew G. Webb (second row, right) received his Ph.D. degree in Medicinal Chemistry from the University of Cambridge in 1990 under Professor Laurie Hall. He was a postdoctoral researcher in the Department of Radiology at the University of Florida before joining the faculty in the Department of Electrical and Computer Engineering at the University of Illinois at Urbana−Champaign.He is currently an Associate Professor, with a full appointment in The Beckman Institute for Advanced Science and Technology. His research areas include the design of microcoils for NMR of mass-limited samples, the use of MRI temperature mapping for hyperthermia, and human brain mapping using functional MRI. Jonathan V. Sweedler (second row, left) received his Ph.D. degree in Analytical Chemistry from the University of Arizona in 1989 under Professor M. Bonner Denton and then spent 3 years at Stanford with Professors Richard Zare and Richard Scheller developing new methods to study neurotransmitters in individual neurons. He is currently a Professor of Chemistry, Neuroscience, and of the Beckman Institute for Advanced Science and Technology at the University of Illinois. His current research interests are twofold: first, he is developing information-rich methods with improved mass sensitivity for nanoliter-volume samples, including microcoil NMR, mass spectrometric imaging, and capillary-scale separations. In addition, he applies these techniques to understanding the role of neurotransmitter and neuropeptide co-transmission and the regulation of behavior in well-defined neuronal networks of opisthobranch molluscs.
“…The commercialisation of the Cold Probes or CryoProbes, including the recent launches of the CryoFlowProbe and Cold Probe with IFC, have made increased NMR sensitivity a reality (Shockcor et al, 1994;Bringmann et al, 2000;Russell et al, 2000;Sigvardson et al, 2002;Spraul et al, 2003). Whilst the costs of purchasing and maintaining these probes may have been prohibitive for many laboratories, the sensitivity enhancements gained truly offer structure elucidation using only microgram amounts of a natural product.…”
Section: Introductionmentioning
confidence: 99%
“…, the 5 mm Cold Probe™ and CryoProbe™ (Shockcor et al, 1994;Bringmann et al, 2000;Russell et al, 2000;Sigvardson et al, 2002), the 3 mm MicroCryoProbe™ (www.bruker-biospin.com/nmr/products/crp.html), and HPLC-NMR with either a CryoFlowProbe™ probe or an interchangeable flow cell (IFC) Cold Probe . In 1995, the Nano probes were reported to yield acceptable 1 H-NMR spectra with 20 µg of a compound (Manzi et al, 1995).…”
Employing a capillary-scale NMR probe enables the miniaturisation of structure determination and de-replication of purified natural products from plants using only 5-100 microg of material. Approximately 5 microg are required to perform one-dimensional proton and two-dimensional homonuclear (COSY and NOESY) NMR experiments; some 30 microg are needed to acquire HMQC- or HSQC-NMR spectra; ca. 75-100 microg are necessary to measure HMBC-NMR spectra; and around 200 microg of a compound are needed to perform 13C- and DEPT-NMR experiments. In order to illustrate the integration of the outputs from high-throughput natural product chemistry methods with the capabilities of the state-of-the-art CapNMR technology, the preparation of a natural product library from the extract of Penstemon centranthifolius, and the subsequent isolation, purification and structure determination of six known iridoid glycosides with 25-300 microg of material are presented.
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