Improved performance and maintenance in gas chromatography/isotope ratio mass spectrometry by precolumn solvent removal.
The crucial step in current concepts to interface isotope ratio mass spectrometry (IRMS) to gas chromatography (GC) is efficient solvent removal. This is due to the essential postcolumn conversion of the analytes into simple gases, which is performed by either combustion or pyrolysis. The capacity of this step merely suffices to convert the analytes. Already small amounts of solvent present in the respective furnace can cause severe damage. In conventional GC/IRMS interfaces, the solvent is removed after passage of the GC column. Either back-flushing or flow diversion is employed for this purpose. Both techniques necessitate the use of numerous components such as unions, tee pieces, valves, and capillary connections. Often this results in significant deterioration of the chromatographic resolution. In contrast, accurate GC/IRMS measurements require baseline separation of adjacent peaks. Moreover, maintenance of conventional interfaces may be tedious and time consuming, mostly because the numerous connections are prone to leakage. In order to avoid these drawbacks, we propose a concept to efficiently remove the solvent before passage of the GC column. It is based on the use of a cooled injection system operated in solvent vent mode, where the solvent elimination is supported by an auxiliary pump. Most unions and tee pieces thus can be removed. The chromatographic resolution is considerably enhanced. In particular, analysis of high-boiling and polar compounds can be improved. At the same time, the maintenance of the system is significantly facilitated. Under the chosen conditions, partial losses of low-boiling analytes during solvent elimination were not associated with significant isotope fractionation.
Flenker
Ulrich
U
Manfred Donike Institute, German Sport University Cologne (DSHS), Carl-Diem-Weg 6, 50933 Cologne, Germany. uli@biochem.dshs-koeln.de
Hebestreit
Moritz
M
Piper
Thomas
T
Hülsemann
Frank
F
Schänzer
Wilhelm
W
D002849:Chromatography, Gas / Q000295:instrumentation* / Q000379:methods*; D007554:Isotopes; D013058:Mass Spectrometry / Q000295:instrumentation* / Q000379:methods*; D012997:Solvents / Q000737:chemistry*; D013256:Steroids / Q000737:chemistry; D013696:Temperature
D007554:Isotopes; D012997:Solvents; D013256:Steroids