Instituto de Biología Agrícola de Mendoza (IBAM-CONICET), Facultad de Ciencias Agrarias, Universidad Nacional de Cuyo, Mendoza, Argentina.
Electrophoresis. 2013 Jun;34(12):1836-43. doi: 10.1002/elps.201300117. Epub 2013 May 26.
This article reports a simple methodology using dispersive liquid-liquid microextraction combined with CZE. It has been applied for the simultaneous determination of phenolic compounds such as caffeic, gallic, vanillic, syringic, cinnamic, p-coumaric acids and oleuropein, apigenin, luteolin, 3-hydroxytyrosol, and tyrosol, in virgin olive oil (VOO). The optimized extraction conditions for 20 g of VOO were: extractant solvent: 400 μL boric acid 30 mM at pH 9.5; dispersive solvent: 300 μL carbon tetrachloride; vortex: 8 min; centrifugation: 3 min. The composition of the BGE was optimized resulting in the selection of a solution made of 30 mM boric acid at pH 9.5. As a strategy for on-line preconcentration a stacking step was applied, injecting a plug of water before sample injection. The short extraction time, centrifugation and electrophoretic steps allow the selective determination of phenolic compounds in VOO with satisfactory LODs (0.004-0.251 mg/kg), recoveries (89.4-101.0%), and RSD (less than 7.44% in peak area and less than 0.69% in migration time), compatible with the concentration levels present in the samples.
本文报道了一种使用分散液-液微萃取结合 CZE 的简单方法。该方法已应用于同时测定橄榄油中的酚类化合物,如咖啡酸、没食子酸、香草酸、丁香酸、肉桂酸、对香豆酸和橄榄苦苷、芹菜素、木犀草素、3-羟基酪醇和酪醇。优化的 20 g 橄榄油萃取条件为:萃取溶剂:400 μL 硼酸 30 mM,pH 9.5;分散溶剂:300 μL 四氯化碳;涡旋:8 min;离心:3 min。优化了 BGE 的组成,选择了 30 mM 硼酸 pH 9.5 的溶液。作为在线浓缩的策略,在进样前注入一段水。短的萃取时间、离心和电泳步骤允许选择性地测定橄榄油中的酚类化合物,具有令人满意的检出限(0.004-0.251 mg/kg)、回收率(89.4-101.0%)和 RSD(峰面积小于 7.44%,迁移时间小于 0.69%),与样品中的浓度水平兼容。