Unit of Food Science and Nutrition, Department of Medicine, Università Campus Bio-Medico di Roma, Rome, Italy.
Department of Chemistry, University of Rome "La Sapienza", Roma, Italy.
Electrophoresis. 2020 Oct;41(20):1752-1759. doi: 10.1002/elps.201900423. Epub 2020 Mar 9.
A HPLC-DAD/ESI-MS method has been developed and validated for the analysis of the most representative phenolic compounds in extra-virgin olive oil (EVOO) samples using a green extraction approach based on deep eutectic solvents (DESs) at room temperature. We examined ten DESs based on choline chloride and betaine in combination with different hydrogen bond donors comprising six alcohols, two organic acids, and one urea. Five phenolic compounds, belonging to the classes of secoiridoids and phenolic alcohols, were selected for the evaluation of extraction efficiency. A betaine-based DES with glycerol (molar ratio 1:2) was found to be the most effective for extracting phenolic compounds as compared to a conventional solvent. The optimization of the extraction method involved the study of the quantity of water to be added to the DES and evaluation of the sample-to-solvent ratio optimal condition. Thirty percent of water added to DES and sample to solvent ratio 1:1 (w/v) were selected as the best conditions. The chromatographic method was validated by studying LOD, LOQ, intraday and interday retention time precision, and linearity range. Recovery values obtained spiking seed oil sample aliquots with standard compounds at 5 and 100 μg/g concentration were in the range between 75.2% and 98.7%.
建立并验证了一种高效液相色谱-二极管阵列检测/电喷雾串联质谱法（HPLC-DAD/ESI-MS），用于分析基于室温深共熔溶剂（DESs）的绿色提取方法提取的特级初榨橄榄油（EVOO）样品中最具代表性的酚类化合物。我们考察了 10 种基于氯化胆碱和甜菜碱的 DES，其中包含 6 种醇、2 种有机酸和 1 种脲，作为不同氢键供体。选择 5 种酚类化合物（属于西奥里多苷类和酚醇类）用于评估提取效率。与常规溶剂相比，发现甘氨酸甜菜碱 DES（摩尔比 1:2）对酚类化合物的提取效果最佳。优化提取方法涉及研究 DES 中添加水的量以及评估最佳的样品与溶剂比条件。选择添加 30% DES 中的水和样品与溶剂比 1:1（w/v）作为最佳条件。通过研究检测限（LOD）、定量限（LOQ）、日内和日间保留时间精密度以及线性范围对色谱方法进行了验证。在 5 和 100 μg/g 浓度下，用标准化合物对种子油样品进行加标，得到的回收率在 75.2%至 98.7%之间。
