Very fast GC analyses are commonly carried out by using 10 m × 0.1 mm id capillaries. In order to achieve rapid elution times (1-3 min), the latter are operated under suboptimum conditions. The present research is focused on the evaluation of use of a 0.1 mm id polar column segment (2 m), operated under near-to-optimum conditions, in very fast GC analysis. The results attained are compared with those derived from using a 10 m microbore column in very fast GC experiments. Prior to method development, the effects of gas velocity, temperature program rate, and sample amounts on analytical performance were evaluated. Following these preliminary applications, a complex lipidic sample, cod liver oil, was subjected to rapid separation (∼2.1 min) on the 10 m capillary through the application of a 50° C/min temperature rate and a 130 cm/ s gas velocity. The same matrix was analyzed on the 2 m capillary using the same temperature program rate and range, but with a close-to-ideal linear velocity. The results observed were of interest, as the separation was achieved in less time (1.45 min) with improved peak resolution. Finally, both methods were validated in terms of retention time and peak area repeatability, LOQ and linearity. © 2008 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.
Evaluation of use of a very short polar microbore column segment in high-speed gas chromatography analysis
TRANCHIDA, Peter Quinto;SCIARRONE, Danilo;DUGO, Paola;MONDELLO, Luigi
2008-01-01
Abstract
Very fast GC analyses are commonly carried out by using 10 m × 0.1 mm id capillaries. In order to achieve rapid elution times (1-3 min), the latter are operated under suboptimum conditions. The present research is focused on the evaluation of use of a 0.1 mm id polar column segment (2 m), operated under near-to-optimum conditions, in very fast GC analysis. The results attained are compared with those derived from using a 10 m microbore column in very fast GC experiments. Prior to method development, the effects of gas velocity, temperature program rate, and sample amounts on analytical performance were evaluated. Following these preliminary applications, a complex lipidic sample, cod liver oil, was subjected to rapid separation (∼2.1 min) on the 10 m capillary through the application of a 50° C/min temperature rate and a 130 cm/ s gas velocity. The same matrix was analyzed on the 2 m capillary using the same temperature program rate and range, but with a close-to-ideal linear velocity. The results observed were of interest, as the separation was achieved in less time (1.45 min) with improved peak resolution. Finally, both methods were validated in terms of retention time and peak area repeatability, LOQ and linearity. © 2008 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.Pubblicazioni consigliate
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