Optimized use of a 50mum ID secondary column in comprehensive two-dimensional gas chromatography-mass spectrometry.
The objective of the present research is directed towards the optimized use of a 50microm ID secondary column, in a comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (GCxGC-qMS) system. The analytical aim was achieved by exploiting a split-flow GCxGC approach, and a rapid-scanning qMS instrument. The stationary phase combination consisted of an apolar (silphenylene polymer) 30mx0.25mm ID column, linked by means of a Y-union, to an MS-connected 1mx0.05mm ID polar one [poly(ethyleneglycol)], and to a 0.20mx0.05mm ID uncoated capillary segment; the latter was connected to a manually operated split-valve. It will be herein demonstrated that the split-flow GCxGC approach, successfully employed in previous H(2)-based, flame ionization detection experiments, provides equally satisfactory results using mass spectrometric detection and helium as carrier gas. An optimized split-flow GCxGC-qMS method was developed and exploited for the analysis of a perfume sample. The results attained were compared with those observed using the same analytical column combination, but with no flow-splitting. It was found that it is not convenient to employ a 50microm ID secondary column in a conventional GCxGC-MS instrument. On the contrary, the use a 50microm ID secondary column, in a split-flow, twin-oven system, provided a good performance. A recently developed comprehensive chromatography software was used for data processing.
Dipartimento Farmaco-chimico, Facoltà di Farmacia, Università di Messina, Viale Annunziata, 98168 Messina, Italy.
Peter Quinto
PQ
Tranchida
Giorgia
G
Purcaro
Chiara
C
Fanali
Paola
P
Dugo
Giovanni
G
Dugo
Luigi
L
Mondello
D008401:Gas Chromatography-Mass Spectrometry / Q000295:instrumentation* / Q000379:methods; D010316:Particle Size; D010476:Perfume / Q000032:analysis; D012117:Resins, Synthetic / Q000737:chemistry*
D010476:Perfume; D012117:Resins, Synthetic