The analysis of complex real-world samples of vegetable origin requires rapid and accurate routine methods, enabling laboratories to increase sample throughput and productivity while reducing analysis costs. This study examines shortening enantioselective-GC (ES-GC) analysis time following the approaches used in fast GC. ES-GC separations are due to a weak enantiomer-CD host–guest interaction and the separation is thermodynamically driven and strongly influenced by temperature. As a consequence, fast temperature rates can interfere with enantiomeric discrimination; thus the use of short and/or narrow bore columns is a possible approach to speeding-up ES-GC analyses. The performance of ES-GC with a conventional inner diameter (I.D.) column (25m length×0.25mm I.D., 0.15m and 0.25m df) coated with 30% of 2,3-di-O-ethyl-6-O-tert-butyldimethylsilyl--cyclodextrin in PS-086 is compared to those of conventional I.D. short column (5m length×0.25mm I.D., 0.15m df) and of different length narrow bore columns (1, 2, 5 and 10mlong×0.10mmI.D., 0.10mdf) in analysing racemate standards of pesticides and in the flavour and fragrance field and real-world-samples. Short conventional I.D. columns gave shorter analysis time and comparable or lower resolutions with the racemate standards, depending mainly on analyte volatility. Narrow-bore columns were tested under different analysis conditions; they provided shorter analysis time and resolutions comparable to those of conventional I.D. ES columns. The narrow-bore columns offering the most effective compromise between separation efficiency and analysis time are the 5 and 2m columns; in combination with mass spectrometry as detector, applied to lavender and bergamot essential oil analyses, these reduced analysis time by a factor of at least three while separation of chiral markers remained unaltered.
Conventional and narrow bore short capillary columns with cyclodextrin derivatives as chiral selectors to speed-up enantioselective gas chromatography and enantioselective gas chromatography–mass spectrometry analyses
BICCHI, Carlo;LIBERTO, Erica;CAGLIERO, Cecilia Lucia;CORDERO, Chiara Emilia Irma;SGORBINI, Barbara;RUBIOLO, Patrizia
2008-01-01
Abstract
The analysis of complex real-world samples of vegetable origin requires rapid and accurate routine methods, enabling laboratories to increase sample throughput and productivity while reducing analysis costs. This study examines shortening enantioselective-GC (ES-GC) analysis time following the approaches used in fast GC. ES-GC separations are due to a weak enantiomer-CD host–guest interaction and the separation is thermodynamically driven and strongly influenced by temperature. As a consequence, fast temperature rates can interfere with enantiomeric discrimination; thus the use of short and/or narrow bore columns is a possible approach to speeding-up ES-GC analyses. The performance of ES-GC with a conventional inner diameter (I.D.) column (25m length×0.25mm I.D., 0.15m and 0.25m df) coated with 30% of 2,3-di-O-ethyl-6-O-tert-butyldimethylsilyl--cyclodextrin in PS-086 is compared to those of conventional I.D. short column (5m length×0.25mm I.D., 0.15m df) and of different length narrow bore columns (1, 2, 5 and 10mlong×0.10mmI.D., 0.10mdf) in analysing racemate standards of pesticides and in the flavour and fragrance field and real-world-samples. Short conventional I.D. columns gave shorter analysis time and comparable or lower resolutions with the racemate standards, depending mainly on analyte volatility. Narrow-bore columns were tested under different analysis conditions; they provided shorter analysis time and resolutions comparable to those of conventional I.D. ES columns. The narrow-bore columns offering the most effective compromise between separation efficiency and analysis time are the 5 and 2m columns; in combination with mass spectrometry as detector, applied to lavender and bergamot essential oil analyses, these reduced analysis time by a factor of at least three while separation of chiral markers remained unaltered.File | Dimensione | Formato | |
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JChromA1212(2008)114_fastESGC.pdf
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