Department of Science and Technology, Soka University, 1-236 Tangi-machi, Hachioji City, Tokyo 192-8577, Japan.
Department of Environmental Engineering for Symbiosis, Graduate School of Engineering, Soka University, 1-236 Tangicho, Hachioji, Tokyo 192-8577, Japan.
Molecules. 2019 Nov 7;24(22):4040. doi: 10.3390/molecules24224040.
Sterols are widely distributed in nature from lipids in organisms to sediments. As a conventional method, extraction and derivatization with TMS have been applied for sterol analysis, requiring a long preparation time for gas chromatography-mass spectrometry analysis. In this study, for sterol analysis, thermochemolysis using tetramethylammonium hydroxide (TMAH) was applied. This method performs hydrolysis and methylation simultaneously; thus, free and ether-bonding sterols can be analyzed as sterol methyl ethers in a relatively short time period. A sediment sample from a tideland (the Yatsu tideland, Japan) was analyzed using the TMAH method, and we detected more than 10 sterols, which include cholest-5-en-3-ol (cholesterol), 24-ethylcholest-5-en-3-ol (sitosterol), 24-methylcholesta-5,22-3-ol (brassicasterol), 24-ethylcholesta-5,24(28)-dien-3-ol (isofucosterol), 4,23,24-trimethyl-5(H)-cholest-22-en-3- ol (dinosterol), and 5(H)-cholestan-3-ol (coprostanol). The detection of the various sterols can be attributed to multiple natural and artificial sources around the Yatsu tideland. In this paper, the mass spectra of these sterols are provided together with an interpretation of their fragmentation patterns. Additionally, the fecal pollution in the Yatsu tideland is discussed in the context of the detection of coprostanol.
甾醇广泛存在于生物体中的脂质和沉积物中。作为一种传统方法，用 TMS 进行提取和衍生化已被应用于甾醇分析，这需要很长的气相色谱-质谱分析准备时间。在这项研究中，用于甾醇分析，采用四甲基氢氧化铵（TMAH）进行热化学分解。该方法同时进行水解和甲基化；因此，游离和醚键结合的甾醇可以作为甾醇甲酯在相对较短的时间内进行分析。使用 TMAH 方法分析了来自潮滩（日本安良岬潮滩）的沉积物样品，我们检测到了 10 多种甾醇，包括胆甾-5-烯-3-醇（胆固醇）、24-乙基胆甾-5-烯-3-醇（谷甾醇）、24-甲基胆甾-5,22-3-醇（菜油甾醇）、24-乙基胆甾-5,24(28)-二烯-3-醇（异福甾醇）、4,23,24-三甲基-5(H)-胆甾-22-烯-3-醇（豆甾醇）和 5(H)-胆甾烷-3-醇（粪甾醇）。在安良岬潮滩周围存在多种天然和人工来源，这导致了各种甾醇的检测。本文提供了这些甾醇的质谱图，并对其碎片模式进行了解释。此外，还根据粪甾醇的检测情况讨论了安良岬潮滩的粪便污染问题。
