Development of Directly Coupled Supercritical Fluid Chromatography-Mass Spectrometry with Self-Spouting and Vacuum Nebulizing Assisted Interface

Abstract

Supercritical fluid chromatograph (SFC) with a fused silica separation column (0.5 mm I.D.x70 cm) packed with ODS-Q3 (30-50 µm) was directly coupled with a quadrupole mass spectrometer (MS) through a vacuum nebulizing interface originally developed for the combination of high performance liquid chromathograph (HPIC) with MS. Mixtures of hexane and ethanol were used as the mobile phase for SFC at a flow rate of 40 µl/min (50 kg/cm2). The column temperatures were maintained above the critical ones of the mobile phase between 260 and 280°C.Introduction of line filters to remove possible small particles in the SFC effluent and the subtle control of the optimum flow and/or the pressure for the SFC column enabled fairly long term stable operation for this SFC-MS system. Thus developed new system was successfully applied to the analysis of various samples such as styrene oligomers, phthalates, triglycerides, and polyethylene glycol derivatives.

Supercritical fluid chromatographic determination of fatty acids and their esters on an ODS-silica gel column

“…The separation and detection of free fatty acids in simple mixtures by SFC/Fourier transform infrared detection were carried out on packed columns using supercritical C02 and Freon 23 as a mobile phase (7). Packed column SFC directly coupled with a mass spectrometer was applied to triglycerides (8). Free fatty acids were separated on an ODS-silica column using a modifier control column containing formic acid installed before a injector and were detected by FID (9).…”

Capillary and packed column SFC/MS

“…This interface allowed flow rates of 60-loop1 min-I to be handled and solvent moderated CI mass spectra were obtained from a range of polar compounds. Use of a LC/MS self-spouting vacuum nebulizing interface has also been described for SFC/MS using packed small bore fused silica columns [14].…”

Rapid determination of phthalates in paper products by supercritical fluid chromatography/tandem mass spectrometry

“…However, the use of UV and light scattering detectors described in these papers did not allow for achieving the highest sensitivity -the LODs of PAEs were at the level of mg/L. Although SFC-MS was earlier proposed for the PAE analysis [30][31][32] and provided two orders of magnitude decrease in LODs, this technique is still not widely used for this type of analytes. It is not surprising that we could not find any references to the use of SFC-MS/MS as the most suitable alternative to HPLC-MS/MS for the analysis of PAEs in pulp and paper products.…”