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Development of fast enantioselective gas-chromatographic analysis using gas-chromatographic method-translation
Carlo Bicchi1, Leonid Blumberg, Cecilia Cagliero
1Dipartimento di Scienza e Tecnologia del Farmaco, Facoltà di Farmacia, Università degli Studi di Torino, Via Pietro Giuria 9, Turin 10125, Italy. carlo.bicchi@unito.it
Abstract:
The study aimed to find the best trade-off between separation of the most critical peak pair and analysis time, in enantioselective GC-FID and GC-MS analysis of lavender essential oil, using the GC method-translation approach. Analysis conditions were first optimized for conventional 25 m x 0.25 mm inner diameter (dc) column coated with 6(I-VII)-O-tert-butyldimethylsilyl-2(I-VII)-3(I-VII)-O-ethyl-beta-cyclodextrin (CD) as chiral stationary phase (CSP) diluted at 30% in PS086 (polymethylphenylpolysiloxane, 15% phenyl), starting from routine analysis. The optimal multi-rate temperature program for a pre-set column pressure was determined and then used to find the pressures producing the efficiency-optimized flow (EOF) and speed-optimized flow (SOF). This method was transferred to a shorter narrow-bore (NB) column (11 m x 0.10 mm) using method-translation software, keeping peak elution order and separation. Optimization of the enantioselective GC method with the translation approach markedly reduced the analysis time of the lavender essential oil, from about 87 min with the routine method to 40 min with an optimal multi-rate temperature program and initial flow with a conventional inner diameter column, and to 15 min with FID as detector or 13.5 min with MS with a corresponding narrow-bore column, while keeping enantiomer separation and efficiency.
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