Nuclear Magnetic Resonance Unit, Scientific Instrumentation Center, University of Granada, Granada, Spain.
Department of Organic Chemistry, University of Granada, Campus Fuentenueva s/n, Granada, Spain.
J Sep Sci. 2018 Dec;41(23):4272-4280. doi: 10.1002/jssc.201800677. Epub 2018 Oct 23.
An analytical method for the analysis of relevant secoiridoid-based components in olive oil, oleacein and oleuropein aglycone, is described using for the first time deuterated surrogates. 0.2 g of sample was necessary to perform the analysis using liquid-liquid extraction and ultrasound-assisted extraction with a mixture of methanol/water (4:1, v/v). To avoid the formation of by-products, normal-phase ultra high performance liquid chromatography was chosen for the chromatographic separation. The selected mobile phase was a gradient mixture of tetrahydrofurane and hexane, and an ACE Excel 3 CN-ES column as stationary phase. The detection and quantification was performed with a SYNAPT G2-Si mass spectrometer. The calibration curves for oleacein and oleuropein aglycone were linear and quadratic, respectively. The validation was done at three levels of concentration. Relative errors from 0.1 to 10.5% and relative standard deviations lower than 9% were obtained. The method was applied to study different samples of olive oil.
本文首次使用氘代内标物描述了橄榄油中相关环烯醚萜类成分（橄榄苦苷和橄榄苦苷元）的分析方法。采用液液萃取和超声辅助提取法（甲醇/水，4:1，v/v），样品用量为 0.2g。为避免副产物的形成，选择正相超高效液相色谱法进行色谱分离。所选流动相为四氢呋喃和正己烷的梯度混合液，以 ACE Excel 3 CN-ES 柱为固定相。采用 SYNAPT G2-Si 质谱仪进行检测和定量。橄榄苦苷和橄榄苦苷元的校准曲线分别为线性和二次曲线。在三个浓度水平进行验证。相对误差为 0.1%至 10.5%，相对标准偏差低于 9%。该方法应用于不同橄榄油样品的研究。
