Packed-column supercritical fluid chromatography/mass spectrometry via a two-stage momentum separator.
J Chromatogr Sci
; 27(6): 274-82, 1989 Jun.
Article
em En
| MEDLINE
| ID: mdl-2738147
ABSTRACT
The practical utility of a two-stage momentum separator for combining packed-column supercritical fluid chromatography (SFC) with mass spectrometry (MS) is described. A Hewlett-Packard model 1084B liquid chromatograph modified for packed-column SFC is connected to a linear fused-silica capillary restrictor housed in a heated probe held at 60 degrees at the terminus. A makeup of coaxial helium gas (1.5 L/min) or dissolved solvent (0.2-0.4 mL/min) can be introduced at the point of supercritical fluid expansion. The latter SFC effluent (0.3-2.0 mL/min) is expanded into a heated (44 degrees) desolvation chamber and directed through a nozzle positioned at the entrance of a two-stage momentum separator. Enrichment of the analyte relative to the volatile gases allows the transfer of sample particles to the MS ion source to produce electron ionization of flash-volatilized eluates. On-line SFC/MS separation and detection of low microgram levels of involatile, thermally labile analytes in synthetic mixtures is accomplished. Identification of an unknown compound in a drug tampering incident and the identification of an unknown metabolite isolated from horse urine is also accomplished.
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Base de dados:
MEDLINE
Assunto principal:
Espectrometria de Massas
/
Cromatografia Líquida de Alta Pressão
Limite:
Animals
Idioma:
En
Revista:
J Chromatogr Sci
Ano de publicação:
1989
Tipo de documento:
Article