Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy.
Chromaleont S.R.L., c/o Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy.
Anal Bioanal Chem. 2022 Jul;414(17):4821-4836. doi: 10.1007/s00216-022-04105-4. Epub 2022 May 10.
Oxygen heterocyclic compounds are secondary metabolites mainly present in the non-volatile fraction of cold-pressed Citrus essential oils. Under this denomination are included coumarins, furocoumarins, and polymethoxyflavones. These compounds possess numerous beneficial properties for human health, but the ingestion of large amounts of coumarins is often related to toxic effects, whereas the phototoxicity caused by furocoumarins and UVA exposure has been well known for a long time. This research has been aimed at the validation of an analytical approach, based on supercritical fluid chromatography coupled to tandem mass spectrometry, for the analysis of OHCs in Citrus essential oils. Among eight columns tested, packed with different stationary phases, the pentafluorophenyl allowed the best baseline separation in 8 min and by using less than 10% of methanol. Calibration curves of twenty-eight standards (coumarins, furocoumarins, polymethoxyflavones) were constructed on spiked lemon distilled essential oil and the method was validated according to the EURACHEM guidelines, by calculating linearity, limit of detection (LoD), limit of quantification (LoQ), accuracy, intra-day, and inter-day precision. Specifically, recoveries were in the 80.0-118.6% range, regression coefficients were between 0.9904 and 0.9998, the LoDs were in the 0.0004-0.0470 mg kg range, the LoQs were in the 0.0014-0.1536 mg kg range, and coefficients of variation were between 0.3 and 2.6% (intra-day) and 1.1 and 7.4% (inter-day). The quantitative profiles of thirteen cold-pressed Citrus essential oils were determined.
氧杂环化合物是次生代谢物，主要存在于冷压柑橘精油的非挥发性部分。在这个命名下包括香豆素、呋喃香豆素和多甲氧基黄酮。这些化合物对人类健康具有许多有益的特性，但大量摄入香豆素通常与毒性作用有关，而呋喃香豆素和 UVA 暴露引起的光毒性长期以来已为人所知。本研究旨在验证一种基于超临界流体色谱与串联质谱联用的分析方法，用于分析柑橘精油中的 OHCs。在测试的八种柱中，填充了不同固定相的五氟苯基柱在 8 分钟内实现了最好的基线分离，且仅使用了不到 10%的甲醇。在柠檬蒸馏精油中添加二十八种标准品（香豆素、呋喃香豆素、多甲氧基黄酮）的校准曲线，并根据 EURACHEM 指南进行方法验证，计算线性、检测限 (LoD)、定量限 (LoQ)、准确度、日内和日间精密度。具体而言，回收率在 80.0-118.6%范围内，回归系数在 0.9904 至 0.9998 之间，LOD 在 0.0004-0.0470mgkg 范围内，LOQ 在 0.0014-0.1536mgkg 范围内，变异系数在 0.3-2.6%（日内）和 1.1-7.4%（日间）之间。确定了十三种冷压柑橘精油的定量图谱。
