Institute of Food Chemistry (170B), University of Hohenheim, Garbenstraße 28, 70599, Stuttgart, Germany.
Anal Bioanal Chem. 2022 Jan;414(2):1061-1071. doi: 10.1007/s00216-021-03730-9. Epub 2021 Oct 30.
Sterols are a highly complex group of lipophilic compounds present in the unsaponifiable matter of virtually all living organisms. In this study, we developed a novel gas chromatography with mass spectrometry selected ion monitoring (GC/MS-SIM) method for the comprehensive analysis of sterols after saponification and silylation. A new referencing system was introduced by means of a series of saturated fatty acid pyrrolidides (FAPs) as internal standards. Linked with retention time locking (RTL), the resulting FAP retention indices (RI) of the sterols could be determined with high precision. The GC/MS-SIM method was based on the parallel measurement of 17 SIM ions in four time windows. This set included eight molecular ions and seven diagnostic fragment ions of silylated sterols as well as two abundant ions of FAPs. Altogether, twenty molecular ions of C- to C-sterols with 0-3 double bonds were included in the final method. Screening of four common vegetable oils (sunflower oil, hemp oil, rapeseed oil, and corn oil) enabled the detection of 30 different sterols and triterpenes most of which could be identified.
甾醇是一类高度复杂的亲脂性化合物,存在于几乎所有生物体的不可皂化物中。在这项研究中,我们开发了一种新的气相色谱-质谱选择离子监测(GC/MS-SIM)方法,用于在皂化和硅烷化后对甾醇进行综合分析。通过一系列饱和脂肪酸吡咯烷(FAP)作为内标,引入了一种新的参考系统。与保留时间锁定(RTL)相结合,可以精确确定甾醇的 FAP 保留指数(RI)。GC/MS-SIM 方法基于在四个时间窗口中对 17 个 SIM 离子进行平行测量。该组包括 8 个分子离子和 7 个硅烷化甾醇的诊断碎片离子以及 2 个 FAP 的丰富离子。总共包括 20 个具有 0-3 个双键的 C 至 C-甾醇的分子离子,最终方法中包括了这些分子离子。对四种常见植物油(葵花籽油、大麻籽油、菜籽油和玉米油)进行筛选,可检测到 30 种不同的甾醇和三萜,其中大多数可被识别。