Cholesterol oxidation products (COPs) are widely studied because they are likely involved in various chronic and degenerative diseases. The aim of this work was to develop a Fast GC/MS method for COPs analysis and to compare it with a conventional GC/MS method. A mixture of eight COPs standards (7α-hydroxycholesterol, 7β-hydroxycholesterol, 19-hydroxycholesterol (internal standard), 5,6α-epoxycholesterol, 5,6β-epoxycholesterol, cholestanetriol, 7-ketocholesterol and 25-hydroxycholesterol) was silylated and analyzed by Fast GC/MS. A capillary GC column Restek RTX-5 (10 m x 0.1 mm i.d. x 0.1 μm f.t.) coated with 5% diphenyl-polysiloxane was used. The temperature was programmed from 250 to 325°C at 20°C/min. The injector and the ion source temperatures were set at 325°C and 230°C, respectively. Helium was used as carrier gas at 43 cm/s. The injection was performed in the split mode (1:50). The electron energy was 70 eV. A mass range from 50 to 600 m/z was scanned at a rate of 3333 amu/s, which corresponded to 0.2 event time. The method gave a fast (total analysis time= 3.5 min) and satisfactory resolution (R > 1.2) of the COPs standards; the limits of detection and quantitation varied from 2.18 to 5.07 ng/mL and from 6.93 to 16.90 ng/mL, respectively. The interday RSD was < 5.79%, whereas the intraday RSD was < 4.29%, which are similar to those found in conventional GC/MS (< 4.28% and < 5.01%, respectively). COPs recoveries evaluated on spiked mice liver, ranged from 72 to 108% for Fast GC/MS, whereas they varied from 77 to 104% for conventional GC/MS. The analytical performance of the 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 good alternative to conventional GC/MS and evinces its great potential for the analysis of both food and biological samples.

Comparison of Fast GC/MS and conventional GC/MS for the determination of cholesterol oxidation products

CARDENIA, VLADIMIRO;RODRIGUEZ ESTRADA, MARIA TERESA;LERCKER, GIOVANNI
2012

Abstract

Cholesterol oxidation products (COPs) are widely studied because they are likely involved in various chronic and degenerative diseases. The aim of this work was to develop a Fast GC/MS method for COPs analysis and to compare it with a conventional GC/MS method. A mixture of eight COPs standards (7α-hydroxycholesterol, 7β-hydroxycholesterol, 19-hydroxycholesterol (internal standard), 5,6α-epoxycholesterol, 5,6β-epoxycholesterol, cholestanetriol, 7-ketocholesterol and 25-hydroxycholesterol) was silylated and analyzed by Fast GC/MS. A capillary GC column Restek RTX-5 (10 m x 0.1 mm i.d. x 0.1 μm f.t.) coated with 5% diphenyl-polysiloxane was used. The temperature was programmed from 250 to 325°C at 20°C/min. The injector and the ion source temperatures were set at 325°C and 230°C, respectively. Helium was used as carrier gas at 43 cm/s. The injection was performed in the split mode (1:50). The electron energy was 70 eV. A mass range from 50 to 600 m/z was scanned at a rate of 3333 amu/s, which corresponded to 0.2 event time. The method gave a fast (total analysis time= 3.5 min) and satisfactory resolution (R > 1.2) of the COPs standards; the limits of detection and quantitation varied from 2.18 to 5.07 ng/mL and from 6.93 to 16.90 ng/mL, respectively. The interday RSD was < 5.79%, whereas the intraday RSD was < 4.29%, which are similar to those found in conventional GC/MS (< 4.28% and < 5.01%, respectively). COPs recoveries evaluated on spiked mice liver, ranged from 72 to 108% for Fast GC/MS, whereas they varied from 77 to 104% for conventional GC/MS. The analytical performance of the 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 good alternative to conventional GC/MS and evinces its great potential for the analysis of both food and biological samples.
Proceedings of the 36th International Symposium on Capillary Chromatography
230
230
V. Cardenia; M.T. Rodriguez-Estrada; G. Lercker
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Utilizza questo identificativo per citare o creare un link a questo documento: http://hdl.handle.net/11585/116220
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