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Development of a non-aqueous capillary electrophoresis method with UV-visible and fluorescence detection for phenolics compounds in olive oil

机译:紫外可见光和荧光法检测橄榄油中酚类化合物的非水毛细管电泳方法的建立

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摘要

Response surface methodology has been applied to the optimization of a simple and rapid non-aqueous capillary electrophoresis method for the separation and determination of several phenolic compounds belonging to the different families present in olive oil. A Box-Behnken design was employed and a total of 27 experiments were performed using olive oil samples spiked with the phenols and injected directly in the capillary after dilution 1:1 with 1-propanol. Finally, the background electrolyte (BGE) was constituted of 25 mM boric acid and 18 mM KOH in a mixture of 74:26 (v/v) 1-propanol/methanol. The hydrophobicity of the BGE allows its miscibility with the olive oil and, as a consequence, the possibility of characterizing and determining these kinds of compounds in this sample without any pretreatment. A hydrodynamic injection (6 s, -30 mbar) was applied and the separation was carried out using 35 °C and +20 kV of separation temperature and voltage, respectively. A capillary with two detection windows for serial online UV and fluorescence detection was satisfactorily employed. The validation of the method was carried out by setting the calibration curves, and the figures of merit were finally obtained. A lineal relationship between the corrected peak area and concentration and limits of detection in the order of micrograms per milliliter were found.
机译:响应面分析法已被用于优化一种简单,快速的非水毛细管电泳方法,以分离和测定橄榄油中不同家族的几种酚类化合物。采用Box-Behnken设计,使用加有酚的橄榄油样品进行了27个实验,并用1-丙醇按1:1稀释后直接注入毛细管中。最后,背景电解质(BGE)由25 mM的硼酸和18 mM的KOH组成,比例为74:26(v / v)1-丙醇/甲醇。 BGE的疏水性使其可与橄榄油混溶,因此无需任何预处理即可表征和测定样品中这类化合物的可能性。施加流体动力注射(6 s,-30 mbar),并分别使用35°C和+20 kV的分离温度和电压进行分离。令人满意地使用了带有两个检测窗口的毛细管,用于串行在线UV和荧光检测。通过设置校准曲线进行方法的验证,并最终获得品质因数。发现校正后的峰面积和浓度之间的线性关系以及检出限为微克每毫升。

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