title: 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.
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 (25 m length x 0.25 mm I.D., 0.15 microm and 0.25 microm d(f)) coated with 30% of 2,3-di-O-ethyl-6-O-tert-butyldimethylsilyl-beta-cyclodextrin in PS-086 is compared to those of conventional I.D. short column (5m length x 0.25 mm I.D., 0.15 microm d(f)) and of different length narrow bore columns (1, 2, 5 and 10 m long x 0.10 mm I.D., 0.10 microm 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 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.
authors.affiliation: Dipartimento di Scienza e Tecnologia del Farmaco, Università degli Studi di Torino, Via Pietro Giuria 9, 10125 Turin, Italy.
authors.forename: Carlo
authors.initials: C
authors.lastname: Bicchi
authors.forename: Erica
authors.initials: E
authors.lastname: Liberto
authors.forename: Cecilia
authors.initials: C
authors.lastname: Cagliero
authors.forename: Chiara
authors.initials: C
authors.lastname: Cordero
authors.forename: Barbara
authors.initials: B
authors.lastname: Sgorbini
authors.forename: Patrizia
authors.initials: P
authors.lastname: Rubiolo
mesh_terms: D003505:Cyclodextrins / Q000737:chemistry*; D005421:Flavoring Agents / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000191:economics / Q000295:instrumentation* / Q000379:methods*; D010476:Perfume / Q000032:analysis; D013237:Stereoisomerism; D013997:Time Factors; D014835:Volatilization
chemical_list: D003505:Cyclodextrins; D005421:Flavoring Agents; D010476:Perfume