The aim of the present study was to set-up a Fast gas chromatography/mass spectrometry method for the analysis of cholesterol oxidation products (COPs). A silylated mixture of seven oxysterol standards was injected into a Fast GC/MS system. A capillary GC column (10 m × 0.1 mm internal diameter × 0.1 μm film thickness) coated with 95% dimethyl- and 5% diphenyl-polysiloxane, was used. The method gave a fast (total analysis time= 3.5 min) and satisfactory resolution (R > 1.2) of the COPs standards, with a good repeatability and sensitivity, similar to those of conventional GC/MS; recoveries were tested on mice liver. Fast GC/MS method suitability for COPs analysis in food was also tested on an oxidized sardine fillet, which had been previously saponified and purified by NH2 solid phase extraction (SPE); a good repeatability and sensitivity was also obtained. The analytical performance of Fast GC/MS method for the determination of COPs, together with the consequent significant reduction of the analysis time and consumables, demonstrates that Fast GC/MS represents a valid alternative to conventional GC/MS and evinces the great potential of such analytical technique, which could be applied to both food and biological samples.
V. Cardenia, M. T. Rodriguez-Estrada, E. Baldacci, S. Savioli, G. Lercker (2012). Analysis of cholesterol oxidation products by Fast gas chromatography/mass spectrometry. JOURNAL OF SEPARATION SCIENCE, 35(3), 424-430 [10.1002/jssc.201100660].
Analysis of cholesterol oxidation products by Fast gas chromatography/mass spectrometry
CARDENIA, VLADIMIRO;RODRIGUEZ ESTRADA, MARIA TERESA;SAVIOLI, STEFANO;LERCKER, GIOVANNI
2012
Abstract
The aim of the present study was to set-up a Fast gas chromatography/mass spectrometry method for the analysis of cholesterol oxidation products (COPs). A silylated mixture of seven oxysterol standards was injected into a Fast GC/MS system. A capillary GC column (10 m × 0.1 mm internal diameter × 0.1 μm film thickness) coated with 95% dimethyl- and 5% diphenyl-polysiloxane, was used. The method gave a fast (total analysis time= 3.5 min) and satisfactory resolution (R > 1.2) of the COPs standards, with a good repeatability and sensitivity, similar to those of conventional GC/MS; recoveries were tested on mice liver. Fast GC/MS method suitability for COPs analysis in food was also tested on an oxidized sardine fillet, which had been previously saponified and purified by NH2 solid phase extraction (SPE); a good repeatability and sensitivity was also obtained. The analytical performance of Fast GC/MS method for the determination of COPs, together with the consequent significant reduction of the analysis time and consumables, demonstrates that Fast GC/MS represents a valid alternative to conventional GC/MS and evinces the great potential of such analytical technique, which could be applied to both food and biological samples.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.