University of Bordeaux, INRAE, Bordeaux INP, UMR1366 Œnologie, ISVV, F-33140 Villenave d'Ornon, France.
J Agric Food Chem. 2022 Apr 20;70(15):4701-4711. doi: 10.1021/acs.jafc.2c00243. Epub 2022 Apr 11.
The chemical analysis of odorous volatile thiols is intrinsically challenging. Substantial progress has been made in quantitative analysis of targeted thiols at ultra-trace concentrations (ng/L), but lesser analytical attention has been given to the qualitative screening of unknown thiols. This work presents a solid-phase extraction (SPE) method using a silver ion (Ag)-based sorbent to isolate volatile thiols from red wine. This proposed Ag SPE method was effective (recovery: 87-101% for four non-furan thiols and 35-49% for two furan thiols), simple, safe, and greatly reduced artifacts, testifying to its suitability as the sample preparation protocol for a qualitative screening experiment. Separation and detection were conducted using heart-cutting multidimensional gas chromatography coupled to mass spectrometry/olfactometry (H/C MDGC-MS/O). Key parameters including H/C width, main host oven temperature, and cryogenic trapping temperature were investigated for optimal instrument performance. The developed Ag SPE H/C MDGC-MS/O strategy was readily applicable for qualitative screening of odorous volatile thiols in wine, as demonstrated by two case studies.
含硫挥发性有机化合物的化学分析本质上具有挑战性。在痕量（ng/L）水平上对靶向硫醇进行定量分析已经取得了相当大的进展，但对未知硫醇的定性筛选关注较少。本工作提出了一种使用基于银离子（Ag）的吸附剂从红酒中分离挥发性硫醇的固相萃取（SPE）方法。所提出的 Ag SPE 方法有效（四种非糠硫醇的回收率为 87-101%，两种糠硫醇的回收率为 35-49%）、简单、安全，并大大减少了伪影，证明其适合作为定性筛选实验的样品制备方案。采用分段多维气相色谱-质谱/嗅闻联用（H/C MDGC-MS/O）进行分离和检测。研究了 H/C 宽度、主炉腔温度和低温捕集温度等关键参数，以获得最佳的仪器性能。所开发的 Ag SPE H/C MDGC-MS/O 策略可方便地应用于葡萄酒中含硫挥发性有机化合物的定性筛选，两个案例研究证明了这一点。
