Department of Food Science, Alma Mater Studiorum-University of Bologna, Bologna, Italy.
J Sep Sci. 2012 Feb;35(3):424-30. doi: 10.1002/jssc.201100660.
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 NH(2) solid-phase extraction (SPE); a good repeatability and sensitivity was also obtained. 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 valid alternative to conventional GC/MS and evinces the great potential of such an analytical technique, which could be applied for both food and biological samples.
本研究的目的是建立一种快速气相色谱/质谱法来分析胆固醇氧化产物(COPs)。将七种氧化固醇标准品的硅烷化混合物注入快速 GC/MS 系统中。使用的毛细管 GC 柱(10 m×0.1 mm 内径×0.1μm 膜厚)涂有 95%二甲基和 5%二苯基聚硅氧烷。该方法能够快速(总分析时间=3.5 分钟)和令人满意地分离 COPs 标准品(R>1.2),具有良好的重复性和灵敏度,与传统 GC/MS 相似;在小鼠肝脏上测试了回收率。还在先前通过 NH(2)固相萃取(SPE)皂化和纯化的氧化沙丁鱼片上测试了快速 GC/MS 方法用于食品中 COPs 分析的适用性;也获得了良好的重复性和灵敏度。快速 GC/MS 法测定 COPs 的分析性能,以及分析时间和消耗品的显著减少,表明快速 GC/MS 是传统 GC/MS 的有效替代方法,并证明了这种分析技术的巨大潜力,该技术可应用于食品和生物样品。