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采用反相分散液相微萃取-快速分辨液相色谱-紫外可见/质谱联用测定初榨橄榄油中酚类化合物

New reversed phase dispersive liquid-liquid microextraction method for the determination of phenolic compounds in virgin olive oil by rapid resolution liquid chromathography with ultraviolet-visible and mass spectrometry detection.

机构信息

University of Extremadura, Analytical Chemistry Department, Badajoz, Spain.

出版信息

J Chromatogr A. 2013 Oct 25;1313:291-301. doi: 10.1016/j.chroma.2013.06.020. Epub 2013 Jul 11.

Abstract

The determination of phenolic compounds in virgin olive oil using a new reversed phase dispersive liquid-liquid microextraction (RP-DLLME) procedure coupled with rapid resolution liquid chromatography-diode array and mass spectrometry detection (RRLC-DAD-MS) have been performed. A rapid resolution Zorbax Eclipse XDB-C18 column (4.6 mm × 50 mm, 1.8 μm particle size) has been employed and eighteen phenolic compounds belonging to different families have been identified and quantified spending a total time of 26 and 13 min with UV-visible and MS detection, respectively. Response surface methodology has been applied by means of a central composite design for the optimization of the variables affecting the extraction procedure searching for the best recovery. The validation of the methods was performed through the establishment of the external standard calibration curves and the analytical figures of merit. Limits of detection ranging from 10 to 400 ng mL(-1) and 1 to 200 ng mL(-1) were achieved using UV-visible and MS detection, respectively. The extraction of phenolic compounds from virgin olive oil was performed in a simple and rapid way by RP-DLLME with ethanol:water 60:40 (v/v) as extracting solvent and 1,4-dioxane as disperser solvent. The quantification of the phenolic compounds in virgin olive oils from different olive varieties was carried out by means of the standard addition method and, finally the procedure for the sample treatment was validated using the well established solid phase extraction procedure with Diol cartridges.

摘要

使用一种新的反相分散液液微萃取(RP-DLLME)程序结合快速分辨液相色谱-二极管阵列和质谱检测(RRLC-DAD-MS)测定了特级初榨橄榄油中的酚类化合物。采用了快速分辨 Zorbax Eclipse XDB-C18 柱(4.6mm×50mm,1.8μm粒径),并鉴定和定量了十八种属于不同类别的酚类化合物,使用 UV-可见和 MS 检测分别花费了 26 和 13 分钟的总时间。通过中心复合设计应用响应面法对影响萃取程序的变量进行了优化,以寻找最佳的回收率。通过建立外部标准校准曲线和分析质量指标对方法进行了验证。使用 UV-可见和 MS 检测,检测限分别为 10-400ng/mL 和 1-200ng/mL。通过 RP-DLLME 用乙醇:水 60:40(v/v)作为萃取溶剂和 1,4-二恶烷作为分散溶剂,从特级初榨橄榄油中简单快速地萃取酚类化合物。通过标准添加法对不同橄榄品种的特级初榨橄榄油中的酚类化合物进行了定量,并最终使用 Diol 小柱的固相萃取程序对样品处理程序进行了验证。

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