Conventional and narrow bore short capillary columns with cyclodextrin derivatives as chiral selectors to speed-up enantioselective gas chromatography and enantioselective gas chromatography–ma

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• 作者：Carlo Bicchi ; Erica Liberto ; Cecilia Cagliero ; Chiara Cordero ; Barbara Sgorbini ; Patrizia Rubiolo
• 关键词：Fast enantioselective GC– ; MS ; Cyclodextrin derivatives ; Linear retention indices ; Mass spectra ; Flavours ; Fragrances
• 刊名：Journal of Chromatography A
• 出版年：2008
• 出版时间：28 November 2008
• 年：2008
• 卷：1212
• 期：1-2
• 页码：114-123
• 全文大小：1377 K

文摘

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 (25 m length × 0.25 mm I.D., 0.15 μm and 0.25 μm d_f) coated with 30 % of 2,3-di-O-ethyl-6-O-tert-butyldimethylsilyl-β-cyclodextrin in PS-086 is compared to those of conventional I.D. short column (5 m length × 0.25 mm I.D., 0.15 μm d_f) and of different length narrow bore columns (1, 2, 5 and 10 m long × 0.10 mm I.D., 0.10 μm d_f) 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 2 m 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.