Pt. Jedrzejewski et Lt. Taylor, EVALUATION OF THE PARTICLE-BEAM INTERFACE FOR PACKED-COLUMN SUPERCRITICAL-FLUID CHROMATOGRAPHY MASS-SPECTROMETRY WITH PURE AND MODIFIED CO2, Journal of chromatography, 677(2), 1994, pp. 365-376
The particle beam interface was evaluated for microbore packed-column
supercritical fluid chromatography-mass spectrometry coupling. The exp
eriments were conducted with mobile phase of pure CO2 and methanol-mod
ified CO2 under flow injection and chromatographic conditions. The eff
ects of various operational parameters were characterized. The electro
n impact limits of detection (LODs) of the system for single ion monit
oring and scan modes were determined to be 5 and 40 ng for caffeine, r
espectively. These LODs are 2.5 to 25 times better than previous repor
ted estimates. Sensitivity was found to be highly dependent on the mod
ifier percentage with 4% methanol-modified CO2 yielding optimal result
s. Separations of phenylurea pesticides and steroids are shown as demo
nstrations of system utility. Background subtracted electron impact sp
ectra were artifact-free and comparable with on-line library spectra.