Linked Life Data

11486859

Source:http://linkedlifedata.com/resource/pubmed/id/11486859

Statements in which the resource exists as a subject.
PredicateObject
rdf:type
lifeskim:mentions
pubmed:issue
1-2
pubmed:dateCreated
2001-8-6
pubmed:abstractText
This paper describes the first coupling of a commercial capillary HPLC system with a diode array spectrophotometric detector and a custom-built nuclear magnetic resonance (NMR) flow microprobe. The eluent from a 3-microm diameter C18 HPLC column is linked to a 500 MHz 1H-NMR microcoil probe with an observe volume of 1.1 microl. The separation and structurally-rich detection of a mixture of terpenoids under both isocratic and gradient solvent elution conditions is presented. The lowest limits of detection yet reported for capillary HPLC on-line measurement (i.e., 37 ng for alpha-pinene) are achieved with this system. The complementary nature of diode array and NMR detection allows stopped-flow data collection from analytes which would otherwise go unnoticed in continuous-flow NMR. Moreover, stopped-flow NMR data is presented for the detection of a trace (sub-nmol) impurity in the sample mixture. Since NMR signals degrade and shift during solvent gradients, flow injection analysis studies are conducted with injected solvent plugs differing in mobile phase composition. The NMR signal degradation accompanying these injections is largely due to the variance in chemical shift with the solvent composition rather than to changes in magnetic susceptibility of the solvent. Characterization of such effects enables the development of improved NMR probes for the coupling of capillary HPLC and NMR.
pubmed:grant
pubmed:language
eng
pubmed:journal
pubmed:citationSubset
IM
pubmed:chemical
pubmed:status
MEDLINE
pubmed:month
Jul
pubmed:issn
0021-9673
pubmed:author
pubmed:issnType
Print
pubmed:day
13
pubmed:volume
922
pubmed:owner
NLM
pubmed:authorsComplete
Y
pubmed:pagination
139-49
pubmed:dateRevised
2009-1-15
pubmed:meshHeading
pubmed:year
2001
pubmed:articleTitle
Union of capillary high-performance liquid chromatography and microcoil nuclear magnetic resonance spectroscopy applied to the separation and identification of terpenoids.
pubmed:affiliation
Department of Chemistry, University of Illinois at Urbana-Champaign, 61801, USA.
pubmed:publicationType
Journal Article, Research Support, U.S. Gov't, P.H.S., Research Support, U.S. Gov't, Non-P.H.S., Research Support, Non-U.S. Gov't