The present paper describes an investigation directed toward the development of a rapid heart-cutting LC-GC method for the analysis of mineral oil saturated hydrocarbons contained in vegetable oils. The automated LC-GC experiments were carried out by using a system equipped with a syringe-type interface, capable of both heart-cutting and comprehensive (LC×GC) two-dimensional analysis. The first dimension separation was achieved on a 100mm×3mm ID×5μm d p silica column, operated under isocratic conditions (hexane). A single 30-s cut, corresponding to a 175μL volume, was transferred to a programmed temperature vaporizer. After the large volume injection, the target analytes were separated in a rapid manner (∼9min) using a 15m×0.1mm ID×0.1μm micro-bore GC capillary. The overall LC-GC run time enables the analysis of ca. 4 samples/hour. Quantification was performed by using external calibration, in the 1-200mg/kg range. The method was validated in terms of linearity, precision, limits of detection and quantification, and accuracy. A series of commercial samples were subjected to analysis. Various degrees of contamination were found in all samples, in the 7.6-180.6mg/kg range.

A rapid multidimensional liquid-gas chromatography method for the analysis of mineral oil saturated hydrocarbons in vegetable oils

PURCARO, Giorgia;CONTE, Lanfranco;MORET, Sabrina;
2011

Abstract

The present paper describes an investigation directed toward the development of a rapid heart-cutting LC-GC method for the analysis of mineral oil saturated hydrocarbons contained in vegetable oils. The automated LC-GC experiments were carried out by using a system equipped with a syringe-type interface, capable of both heart-cutting and comprehensive (LC×GC) two-dimensional analysis. The first dimension separation was achieved on a 100mm×3mm ID×5μm d p silica column, operated under isocratic conditions (hexane). A single 30-s cut, corresponding to a 175μL volume, was transferred to a programmed temperature vaporizer. After the large volume injection, the target analytes were separated in a rapid manner (∼9min) using a 15m×0.1mm ID×0.1μm micro-bore GC capillary. The overall LC-GC run time enables the analysis of ca. 4 samples/hour. Quantification was performed by using external calibration, in the 1-200mg/kg range. The method was validated in terms of linearity, precision, limits of detection and quantification, and accuracy. A series of commercial samples were subjected to analysis. Various degrees of contamination were found in all samples, in the 7.6-180.6mg/kg range.
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Utilizza questo identificativo per citare o creare un link a questo documento: http://hdl.handle.net/11390/868903
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