On‐line reversed‐phase liquid chromatography‐capillary gas chromatography using a programmed temperature vaporizer as interface

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Abstract
An on‐line reversed‐phase LC‐GC method involving the use of a Programmed Temperature Vaporizer (PTV) as interface is used for the rapid analysis of sterols. The experimental procedure requires only the use of commercial HPLC and GC equipments and a Rheodyne valve. The LC preseparation can be performed satisfactorily even with aqueous eluents containing up to 25% water. Factorial experimental design is applied to investigate the sensitivity achievable in the analysis with some variables (adsorbent material used in the PTV, particle size and plug length) being considered at two different levels. As a result, the sensitivty can be increased by a factor as large as 35 merely by performing the analysis under the experimental conditions giving the highest response. The use of the proposed configuration allows the transfer of up to 1050 μL from LC into the GC system, 1400 μL/min being the speed of sample introduction. The proposed procedure was succesfully applied to the analysis of real samples.

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