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Chromatographic separations and liquid phase extraction/concentration of some polyphenolic compounds: a comparison between reverse phase and cation-exchange chromatography

机译:某些多酚化合物的色谱分离和液相萃取/浓缩:反相色谱与阳离子交换色谱的比较

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Chromatographic performance based on the use of a C_(18) reverse phase and a LC-SCX cation-exchange column associated with UV absorption at 280 nm is optimized and compared for the simultaneous determination of resveratrol and other polyphenolic compounds with the aim to establish the best experimental conditions for the trace analysis of these substances. Under the optimized chromatographic conditions using a gradient acid mobile phase and acetonitrile as a modifier solvent, the elution of all injected compounds was completed in about 30 min of analysis and the detection limits (LOD) ranged between 20 nM and 120 nM. The regression analysis for most of the analyzed compounds shows linear ranges spanning over five orders of magnitude with correlation coefficients always £0.98. A liquid-liquid extraction procedure was optimized using three different extracting solvents such as methyl ethyl ketone, diethyl ether, and dichloromethane. The hydrophilic/hydrophobic character of the water/organic solvent was modulated by addition of NaCl salt. In order to ascertain the analytical potentialities of the investigated method, and in particular the performance of the extraction procedure, a wide variety of selected red wines were analysed. The average recoveries ranged between 73% and 103% for the analysed molecules, indicating both the practical absence of interfering peaks on the chromatographic separation and an appreciable capacity of extraction of polyphenolic acids from the wine matrices.
机译:优化并比较了基于C_(18)反相色谱和LC-SCX阳离子交换柱与280 nm处的UV吸收的色谱性能,以便同时测定白藜芦醇和其他多酚化合物,从而建立色谱柱。这些物质的痕量分析的最佳实验条件。在使用梯度酸流动相和乙腈作为改性剂溶剂的优化色谱条件下,所有进样化合物的洗脱均在大约30分钟的分析过程中完成,检测限(LOD)介于20 nM至120 nM之间。对大多数分析化合物的回归分析显示,线性范围跨越五个数量级,相关系数始终为£ 0.98。使用三种不同的萃取溶剂(例如甲乙酮,乙醚和二氯甲烷)优化了液-液萃取程序。通过添加NaCl盐调节水/有机溶剂的亲水/疏水特性。为了确定所研究方法的分析潜力,尤其是确定提取程序的性能,对各种精选的红酒进行了分析。被分析分子的平均回收率在73%至103%之间,这表明在色谱分离过程中实际上不存在干扰峰,并且从葡萄酒基质中提取多酚酸的容量相当大。

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