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Title: Mass spectrometry with direct supercritical fluid injection

Abstract

Direct fluid injection mass spectrometry utilizes supercritical fluids for solvation and transfer of materials to a mass spectrometer chemical ionization (CI) source. Available data suggest that any material soluble in a supercritical fluid is transferred efficiently to the ionization region. Mass spectra are presented for mycotoxins of the trichothecene group obtained by use of supercritical carbon dioxide with isobutane as the CI reagent gas. Direct fluid injection MS/MS is also illustrated for major ions in the isobutane chemical ionization of T-2 toxin. The effect of pressure and temperature upon solubility in supercritical fluids is described and illustrated for diacetoxyscirpenol. A potential method is also demonstrated for ''on-line fractionation'' during MS analysis using pressure to control supercritical fluid solubility. Mass spectra are also presented for polar compounds, using supercritical ammonia, and the extension to complex mixtures is described. The fundamental basis and experimental requirements of the direct fluid injection process are discussed. 1 figure, 11 tables.

Authors:
;
Publication Date:
Research Org.:
Pacific Northwest Lab., Richland, WA
OSTI Identifier:
6972431
DOE Contract Number:
AC06-76RL01830
Resource Type:
Journal Article
Resource Relation:
Journal Name: Anal. Chem.; (United States); Journal Volume: 55:14
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; AMINES; MASS SPECTRA; CHLORINATED AROMATIC HYDROCARBONS; COAL LIQUIDS; MASS SPECTROMETERS; EQUIPMENT INTERFACES; FLUID INJECTION PROCESSES; SUPERCRITICAL FLUID CHROMATOGRAPHY; TOXINS; 2-METHYLPROPANE; AMMONIA; CALIBRATION; CARBON DIOXIDE; CONDENSED AROMATICS; CRITICAL PRESSURE; CRITICAL TEMPERATURE; EXPERIMENTAL DATA; FEASIBILITY STUDIES; FLOW RATE; GASES; HIGH PRESSURE; HIGH TEMPERATURE; MEDIUM PRESSURE; MEDIUM TEMPERATURE; PRESSURE DEPENDENCE; QUALITATIVE CHEMICAL ANALYSIS; REAGENTS; SOLVATION; SOLVENT PROPERTIES; TEMPERATURE DEPENDENCE; TIME DEPENDENCE; ALKANES; ANTIGENS; AROMATICS; CARBON COMPOUNDS; CARBON OXIDES; CHALCOGENIDES; CHEMICAL ANALYSIS; CHROMATOGRAPHY; DATA; FLUIDS; HALOGENATED AROMATIC HYDROCARBONS; HYDRIDES; HYDROCARBONS; HYDROGEN COMPOUNDS; INFORMATION; LIQUIDS; MATERIALS; MEASURING INSTRUMENTS; NITROGEN COMPOUNDS; NITROGEN HYDRIDES; NUMERICAL DATA; ORGANIC CHLORINE COMPOUNDS; ORGANIC COMPOUNDS; ORGANIC HALOGEN COMPOUNDS; OXIDES; OXYGEN COMPOUNDS; PHYSICAL PROPERTIES; SEPARATION PROCESSES; SPECTRA; SPECTROMETERS; THERMODYNAMIC PROPERTIES; TOXIC MATERIALS; TRANSITION TEMPERATURE; 400104* - Spectral Procedures- (-1987)

Citation Formats

Smith, R.D., and Udseth, H.R. Mass spectrometry with direct supercritical fluid injection. United States: N. p., 1983. Web. doi:10.1021/ac00264a016.
Smith, R.D., & Udseth, H.R. Mass spectrometry with direct supercritical fluid injection. United States. doi:10.1021/ac00264a016.
Smith, R.D., and Udseth, H.R. 1983. "Mass spectrometry with direct supercritical fluid injection". United States. doi:10.1021/ac00264a016.
@article{osti_6972431,
title = {Mass spectrometry with direct supercritical fluid injection},
author = {Smith, R.D. and Udseth, H.R.},
abstractNote = {Direct fluid injection mass spectrometry utilizes supercritical fluids for solvation and transfer of materials to a mass spectrometer chemical ionization (CI) source. Available data suggest that any material soluble in a supercritical fluid is transferred efficiently to the ionization region. Mass spectra are presented for mycotoxins of the trichothecene group obtained by use of supercritical carbon dioxide with isobutane as the CI reagent gas. Direct fluid injection MS/MS is also illustrated for major ions in the isobutane chemical ionization of T-2 toxin. The effect of pressure and temperature upon solubility in supercritical fluids is described and illustrated for diacetoxyscirpenol. A potential method is also demonstrated for ''on-line fractionation'' during MS analysis using pressure to control supercritical fluid solubility. Mass spectra are also presented for polar compounds, using supercritical ammonia, and the extension to complex mixtures is described. The fundamental basis and experimental requirements of the direct fluid injection process are discussed. 1 figure, 11 tables.},
doi = {10.1021/ac00264a016},
journal = {Anal. Chem.; (United States)},
number = ,
volume = 55:14,
place = {United States},
year = 1983,
month =
}
  • The application of on-line supercritical fluid extraction with chemical ionization mass spectrometry and collision induced dissociation tandem mass spectrometry for the rapid identification of parts-per-million levels of several trichothecene mycotoxins is demonstrated. Supercritical carbon dioxide is shown to allow identification of mycotoxins with minimum sample handling in complex natural matrices (e.g., wheat). Tandem mass spectrometry techniques are employed for unambiguous identification of compounds of varying polarity, and false positives from isobaric compounds are avoided. Capillary column supercritical fluid chromatography-mass spectrometry of a supercritical fluid extract of the same sample was also performed and detection limits in the parts-per-billion range appearmore » feasible.« less
  • Direct fluid injection mass spectrometry utilizes supercritical fluids for solvation and transfer of materials to a mass spectrometer chemical ionization (CI) source. Available data suggest that any material soluble in a supercritical fluid is transferred efficiently to the ionization region. Mass spectra are presented for mycotoxins of the trichothecene group obtained by use of supercritical carbon dioxide with isobutane as the CI reagent gas. Direct fluid injection MS/MS is also illustrated for major ions in the isobutane chemical ionization of T-2 toxin. The effect of pressure and temperature upon solubility in supercritical fluids is described and illustrated for diacetoxycirpenol. Amore » potential method is also demonstrated for on-line fraction during MS analysis using pressure to control supercritical fluid solubility. Mass spectra are also presented for polar compounds, using supercritical ammonia, and the extension to complex mixtures is described. The fundamental basis and experimental requirements of the direct fluid injection process are discussed. 34 references, 11 figures, 1 table.« less
  • A capillary supercritical fluid chromatograph was occupied to a double focusing mass spectrometer with a direct heated probe interface. The interface contained a fused silica transfer capillary containing a frit restrictor at the end which was heated to a temperature of 300-350/degrees/C by resistance heating. The total column effluent was transferred into the mass spectrometer ion source. This interface not only preserved the chromatographic efficiency but also provided for mass spectral detection and identification of various high molecular weight, thermally labile, and polar compounds. Electron-impact and chemical ionization mass spectra of selected natural products and pharmaceuticals were obtained at themore » low nanogram level.« less
  • A simple electron impact ionization source interface was developed for a combined capillary column supercritical fluid chromatography and mass spectrometry systems (SFC-MS). The sensitivity of the system was illustrated by the analysis of a sample containing 100 pg quantities of 4-aminobiphenyl, benzidine, and 3,3'-dichlorobenzidine. An analysis was also performed of the labile pesticide aldicarb. The latter analysis was performed additionally to determine the thermal effects of the chromatography. The total system was shown to enhance the flexibility of SFC-MS compared to standard liquid chromatography-mass spectrometry.
  • An instrument developed in the author's laboratory and incorporating a capillary column supercritical fluid chromatography (SFC), a direct fluid injection (DFI) interface, and a tandem quadrupole mass spectrometer equipped with a dual electron impact-chemical ionization ion source is described. Initial results of separations suggest excellent separations and sensitivities using the described instrument. Advantages of the capillary SFC-DFI interface are due to the low flow rates, high mobile phase volatility, and the capability for mixed chemical ionization reagents. (BLM)