Department of Chemistry, University of Science and Technology of China.
J Chromatogr A. 2013 Mar 8;1280:122-7. doi: 10.1016/j.chroma.2013.01.028. Epub 2013 Jan 16.
A reliable and simple method for quantitative analysis of free and conjugated neutral aroma components (including aldehydes, ketones, alcohols, esters and alkenes) in tobacco using comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-TOFMS) is described. Simple solvent extraction using methyl tert-butyl ether (MTBE) ensured extraction of the neutral aroma components in their free form. The components present as conjugates were isolated using MTBE extraction following acid-catalysed hydrolysis. The GC × GC-TOFMS analysis was performed to comprehensively identify different forms of neutral aroma components in tobacco. Compared with the conventional methods, our method not only simplified the process but also saved time and solvent. It also exhibited higher selectivity and sensitivity and demonstrated the following results: the limit of detection of the neutral aroma components varied from 0.006 μg/g for 2-acetylfuran to 0.133 μg/g for 5-(hydroxymethyl)-2-furfural, the relative standard deviations were from 0.5% to 6.8% and the recovery ranged from 82.4% to 118.2%. The optimized method was successfully employed to analyse real tobacco samples. Eighty-three neutral aroma components of interest were identified.
描述了一种使用全二维气相色谱-飞行时间质谱（GC×GC-TOFMS）定量分析烟草中游离和结合中性香气成分（包括醛、酮、醇、酯和烯烃）的可靠且简单的方法。使用甲基叔丁基醚（MTBE）进行简单的溶剂萃取可确保游离形式的中性香气成分得到提取。用 MTBE 萃取并在酸催化水解后分离出作为结合物存在的成分。通过 GC×GC-TOFMS 分析可全面鉴定烟草中不同形式的中性香气成分。与传统方法相比，该方法不仅简化了流程，还节省了时间和溶剂。它还表现出更高的选择性和灵敏度，并得到以下结果：中性香气成分的检测限从 2-乙酰呋喃的 0.006μg/g 到 5-羟甲基-2-糠醛的 0.133μg/g 不等，相对标准偏差在 0.5%至 6.8%之间，回收率在 82.4%至 118.2%之间。优化后的方法成功地用于分析实际烟草样品。鉴定出 83 种感兴趣的中性香气成分。
