Nutrition and Bromatology Group, Analytical and Food Chemistry Department, Faculty of Food Science and Technology, University of Vigo, Ourense Campus, E-32004 Ourense, Spain.
Nutrition and Bromatology Group, Analytical and Food Chemistry Department, Faculty of Food Science and Technology, University of Vigo, Ourense Campus, E-32004 Ourense, Spain.
Food Chem. 2014 May 1;150:128-36. doi: 10.1016/j.foodchem.2013.10.157. Epub 2013 Nov 5.
A reliable, sensitive and effective method based on ultrasound-assisted emulsification-microextraction (USAEME) coupled to HPLC-DAD has been developed to identify and quantify several target phenolic compounds from extra virgin olive oils (EVOO). This approach is based on the emulsification of a microvolume of polar organic extractant in a non-polar liquid sample by ultrasound radiation and further separation of both liquid phases by centrifugation. The percentage of methanol/water (v/v) in the extractant, the volume of extractant, and the extraction time as three effective parameters on the extraction were optimised by a central composite design (Box-Behnken response surface) method. The optimised method presented recoveries in EVOO between 91% and 115% for the target analytes (except vanillin with 65%) and a satisfactory precision with relative standard deviations (RSD%) lower than 8.4% for repeatability and reproducibility. The method showed good linearity and limits of detection and quantification were in the range 0.001-0.14 and 0.004-0.47mg/kg, respectively. After method validation, it was successfully applied to the analysis of three EVOO samples. All target compounds were detected in all analysed samples. Tyrosol and hydroxytyrosol were the major phenolic compounds, followed by pinoresinol and luteolin.
建立了一种可靠、灵敏、有效的基于超声辅助乳化-微萃取（USAEME）与高效液相色谱-二极管阵列检测（HPLC-DAD）联用的方法，用于鉴定和定量分析特级初榨橄榄油（EVOO）中的多种目标酚类化合物。该方法基于超声辐射将微体积的极性有机溶剂乳化成非极性液体样品，并通过离心进一步分离两种液相。通过中心复合设计（Box-Behnken 响应面）方法优化了萃取中甲醇/水（v/v）的百分比、萃取剂体积和萃取时间这三个有效参数。优化后的方法在 EVOO 中对目标分析物的回收率在 91%至 115%之间（除香草醛为 65%），并且具有令人满意的精密度，重复性和再现性的相对标准偏差（RSD%）低于 8.4%。该方法表现出良好的线性，检测限和定量限的范围分别为 0.001-0.14 和 0.004-0.47mg/kg。方法验证后，成功应用于三种 EVOO 样品的分析。所有目标化合物均在所有分析样品中被检测到。酪醇和羟基酪醇是主要的酚类化合物，其次是松柏醇和木犀草素。
