Microflow NMR : concepts and capabilities
The principles and parameters to consider when choosing an NMR probe for analysis of a volume- or mass-limited sample are identified and discussed. In particular, a capillary-based microflow probe is described which has a mass sensitivity comparable to cryoprobes (observe volume approximately 40 microL), but with several distinct advantages. The microflow probe has a flowcell volume of 5 microL and an observe volume of 1.5 microL and is equipped with proton and carbon observe channels, deuterium lock, and z-gradient capability. The entire flow path is fused silica; inlet and outlet capillary inner diameters are 50 microm to minimize sample dispersion, making it well-suited to volume-limited samples. An injected sample of 1 nmol of sucrose (0.34 microg in 3 microL, 0.33 mM; MW = 342 g/mol) yields a 1D proton spectrum in 10 min on a spectrometer of 500 MHz or higher. In another example, 15 microg of sucrose (in 3 microL; 15 mM, 45 nmol) is injected and parked in the probe to yield a heteronuclear multiple-quantum coherence (HMQC) spectrum in less than 15 h. The natural product muristerone A (75 microg in 3 microL, 50 mM, 150 nmol; MW = 497 g/mol) was delivered to the flow cell, and a gradient correlation spectroscopy spectrum was acquired in 7 min, a gradient HMQC in 4 h, and a gradient heteronuclear multiple-bond correlation in 11 h. Four basic modes of sample injection into the probe vary in degree of user intervention, speed, solvent consumption, and sample delivery efficiency. Manual, manual-assisted (employing a micropump), automated (using an autosampler), and capillary HPLC modes of operation are described.
| Medienart: |
Artikel |
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| Erscheinungsjahr: |
2004 |
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| Erschienen: |
2004 |
| Enthalten in: |
Zur Gesamtaufnahme - volume:76 |
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| Enthalten in: |
Analytical chemistry - 76(2004), 10 vom: 15. Mai, Seite 2966-74 |
| Sprache: |
Englisch |
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| Beteiligte Personen: |
Olson, Dean L [VerfasserIn] |
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| Themen: |
38778-30-2 |
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| Anmerkungen: |
Date Completed 06.08.2004 Date Revised 14.11.2007 published: Print Citation Status MEDLINE |
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| Förderinstitution / Projekttitel: |
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| PPN (Katalog-ID): |
NLM148343619 |
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| 100 | 1 | |a Olson, Dean L |e verfasserin |4 aut | |
| 245 | 1 | 0 | |a Microflow NMR |b concepts and capabilities |
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| 500 | |a Date Completed 06.08.2004 | ||
| 500 | |a Date Revised 14.11.2007 | ||
| 500 | |a published: Print | ||
| 500 | |a Citation Status MEDLINE | ||
| 520 | |a The principles and parameters to consider when choosing an NMR probe for analysis of a volume- or mass-limited sample are identified and discussed. In particular, a capillary-based microflow probe is described which has a mass sensitivity comparable to cryoprobes (observe volume approximately 40 microL), but with several distinct advantages. The microflow probe has a flowcell volume of 5 microL and an observe volume of 1.5 microL and is equipped with proton and carbon observe channels, deuterium lock, and z-gradient capability. The entire flow path is fused silica; inlet and outlet capillary inner diameters are 50 microm to minimize sample dispersion, making it well-suited to volume-limited samples. An injected sample of 1 nmol of sucrose (0.34 microg in 3 microL, 0.33 mM; MW = 342 g/mol) yields a 1D proton spectrum in 10 min on a spectrometer of 500 MHz or higher. In another example, 15 microg of sucrose (in 3 microL; 15 mM, 45 nmol) is injected and parked in the probe to yield a heteronuclear multiple-quantum coherence (HMQC) spectrum in less than 15 h. The natural product muristerone A (75 microg in 3 microL, 50 mM, 150 nmol; MW = 497 g/mol) was delivered to the flow cell, and a gradient correlation spectroscopy spectrum was acquired in 7 min, a gradient HMQC in 4 h, and a gradient heteronuclear multiple-bond correlation in 11 h. Four basic modes of sample injection into the probe vary in degree of user intervention, speed, solvent consumption, and sample delivery efficiency. Manual, manual-assisted (employing a micropump), automated (using an autosampler), and capillary HPLC modes of operation are described | ||
| 650 | 4 | |a Comparative Study | |
| 650 | 4 | |a Journal Article | |
| 650 | 4 | |a Research Support, U.S. Gov't, P.H.S. | |
| 650 | 7 | |a Protons |2 NLM | |
| 650 | 7 | |a Solvents |2 NLM | |
| 650 | 7 | |a muristerone A |2 NLM | |
| 650 | 7 | |a 38778-30-2 |2 NLM | |
| 650 | 7 | |a Ecdysterone |2 NLM | |
| 650 | 7 | |a 5289-74-7 |2 NLM | |
| 650 | 7 | |a Sucrose |2 NLM | |
| 650 | 7 | |a 57-50-1 |2 NLM | |
| 650 | 7 | |a Carbon |2 NLM | |
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| 700 | 1 | |a Norcross, James A |e verfasserin |4 aut | |
| 700 | 1 | |a O'Neil-Johnson, Mark |e verfasserin |4 aut | |
| 700 | 1 | |a Molitor, Paul F |e verfasserin |4 aut | |
| 700 | 1 | |a Detlefsen, David J |e verfasserin |4 aut | |
| 700 | 1 | |a Wilson, Aaron G |e verfasserin |4 aut | |
| 700 | 1 | |a Peck, Timothy L |e verfasserin |4 aut | |
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