School of Chemical Sciences, The University of Auckland | Waipapa Taumata Rau, Auckland, New Zealand.
School of Chemical Sciences, The University of Auckland | Waipapa Taumata Rau, Auckland, New Zealand; École Nationale Supérieure de Chimie de Mulhouse, Mulhouse, France.
J Chromatogr A. 2023 Sep 27;1707:464273. doi: 10.1016/j.chroma.2023.464273. Epub 2023 Aug 5.
Improvements to the quantification of three white wine impact odorants 3-sulfanylhexan-1-ol, 3-sulfanylhexyl acetate, and 4-sulfanyl-4-methylpentan-2-one, and the non-volatile precursors from which they are released during fermentation, is of great interest to the wine science community. Recent reports of a "Quick, Easy, Cheap, Effective, Rugged and Safe" (QuEChERS) based method for the concurrent analysis of these thiols and their precursors via liquid chromatography tandem mass spectrometry (LC-MS/MS) has enabled the development of far simpler methods, as well as aligning these analyses with principles of green analytical chemistry. This current work reports the development and validation of a QuEChERS based LC-MS/MS method utilising a safer derivatising agent, 4,4'-dithiodipyridine, while greatly minimising the reagents involved and waste produced. We demonstrate that this new method compares favourably to the previously reported method with repeatability of 0.2-1.3%RSD and 0.4-5.2%RSD for precursors and free thiols. Further, the commercially available internal standard, 1-hexanethiol, used in previous analytical methods was compared to stable isotope labelled analogues of the analytes, with results suggesting that it may not be a reliable internal standard.
改进三种白葡萄酒气味影响物（3-巯基己醇、3-巯基己酸乙酯和 4-巯基-4-甲基-2-戊酮）以及发酵过程中释放它们的非挥发性前体的定量分析方法，一直是葡萄酒科学界关注的焦点。最近有报道称，采用“快速、简便、廉价、有效、耐用和安全”（QuEChERS）的方法，通过液相色谱串联质谱（LC-MS/MS）同时分析这些硫醇及其前体，这使得开发更为简单的方法成为可能，并使这些分析方法符合绿色分析化学的原则。本研究报告了一种基于 QuEChERS 的 LC-MS/MS 方法的开发和验证，该方法使用更安全的衍生化试剂 4,4'-二硫代二吡啶，同时大大减少了所需试剂的用量和产生的废物。我们证明，与之前报道的方法相比，这种新方法具有更好的重复性，对于前体和游离硫醇，其重复性分别为 0.2-1.3%RSD 和 0.4-5.2%RSD。此外，之前分析方法中使用的市售内标 1-己硫醇与分析物的稳定同位素标记类似物进行了比较，结果表明它可能不是一种可靠的内标。
