Sha Yunfei, Deng Chunhui, Zhang Haobo, Xie Wenyan, Liu Baizhan
Shanghai Tobacco (Group) Corporation Technical Center, Shanghai, China.
J Sep Sci. 2008 Jul;31(13):2451-6. doi: 10.1002/jssc.200800108.
Ergosterol is one of the important precursors of tumorigenic polynuclear aromatic hydrocarbons. To the best of our knowledge, a large amount of ergosterol is present in moldy cigarettes, which derives from fungal contaminations. Thus, the development of a simple, fast, and efficient method for the analysis of ergosterol is in great demand. In this paper, GC/MS following microwave-assisted silylation (MAS) was developed for the rapid quantitative analysis of ergosterol in cigarettes for the first time. In our work, total ergosterol in cigarettes after NaOH saponification was extracted with hexane, and then was fast derivatized with bis(trimethylsilyl)trifluoroacetamide (BSTFA) under microwave irradiation. Finally, the ergosterol trimethylsilyl derivative was analyzed by GC/MS. Derivatization conditions including microwave reaction solvent, irradiation time, and power were investigated. Method validations (linear range, LOD, precision, and recovery) were also studied. The results showed that the proposed method provided a fast, simple, and sensitive approach for the determination of ergosterol in cigarettes. Finally it was successfully applied to the analysis of ergosterol in normal and mildewy cigarettes.
麦角甾醇是致瘤性多环芳烃的重要前体之一。据我们所知，发霉香烟中存在大量麦角甾醇，其来源于真菌污染。因此，迫切需要开发一种简单、快速且高效的麦角甾醇分析方法。本文首次开发了微波辅助硅烷化（MAS）后气相色谱/质谱联用（GC/MS）法，用于快速定量分析香烟中的麦角甾醇。在我们的工作中，用己烷提取经氢氧化钠皂化后的香烟中总麦角甾醇，然后在微波辐射下用双（三甲基硅基）三氟乙酰胺（BSTFA）进行快速衍生化。最后，通过GC/MS分析麦角甾醇三甲基硅基衍生物。研究了包括微波反应溶剂、辐射时间和功率在内的衍生化条件。还研究了方法验证（线性范围、检测限、精密度和回收率）。结果表明，所提出的方法为测定香烟中的麦角甾醇提供了一种快速、简单且灵敏的方法。最后，该方法成功应用于正常香烟和发霉香烟中麦角甾醇的分析。
