食品科学 ›› 2008, Vol. 29 ›› Issue (4): 283-286.

• 分析检测 • 上一篇    下一篇

固相萃取-高效液相色谱法同时测定葡萄酒中没食子酸等8种多酚类化合物

 李永库, 李晓静, 欧小辉   

  1. 沈阳农业大学理学院; 广西大学糖业工程技术研究中心; 广西大学糖业工程技术研究中心;
  • 出版日期:2008-04-15 发布日期:2011-08-24

Simultaneous Analysis of Eight Phenolic Compounds in Wines by SPE-HPLC-PAD

 LI  Yong-Ku, LI  Xiao-Jing, 欧Xiao-Hui   

  1. 1.College of Science, Shenyang Agricultural University; 2. Center for Sugar Technology Research, Guangxi University
  • Online:2008-04-15 Published:2011-08-24

摘要: 建立了固相萃取-高效液相色谱光电二极管阵列检测法测定葡萄酒中没食子酸等8种多酚类生物活性化合物的方法。并用此方法测定了市售的7种葡萄酒中该8种生物活性物质的含量。实验确定了葡萄酒样品中的没食子酸等物质的固相萃取方法,通过优化萃取条件,有效的去除了葡萄酒中大量干扰成分。采用HypersilC18柱(250mm×4.6mm,i.d.5μm)分离。以乙腈-0.3%乙酸为流动相,线性梯度洗脱,以保留时间和特征光谱对分离出的组分予以定性确证,用峰面积进行定量。8种组分的质量浓度与其峰面积在一定的范围内有良好的线性关系,相关系数为0.9982~0.9999,8种组分的平均回收率为83.9%~103.7%(相对标准偏差为1.6%~4.6%),检测限为0.2~1.5mg/L。对市售的7种葡萄酒的检测结果表明,多酚类物质作为葡萄酒中重要的生物活性成分,其含量与葡萄酒的酿造方式,葡萄品种,葡萄产地有密切的关系。该方法简便、快速、灵敏,也适用于其它复杂体系中没食子酸等8种生物活性的成分分析。

关键词: 固相萃取, 高效液相色谱-二极管阵列检测法, 葡萄酒, 多酚物质

Abstract: A method has been developed for the simultaneous determination of the contents of galic acid, Catechin, (-)- epicatechin, Caffeic acid, pyrocatechol, Chlorogenic acid, flavone and Felinic acid in wines by high performance liquid chroma- tography- photodiode array detector (HPLC-PAD)with solid phase extraction (SPE). The techniques of SPE including the activation of the SPE column, elimination of interference and elution conditions of samples were confirmed. The analytes were separated by using a Hypersil Cl8 column (250 mm×4.6 mm, i.d. 5μm) and acetonitrile-0.3%HAc as mobile phase with linear gradient elution. The eight compounds were identified by retention time data and spectral characteristics and quantified by peak area. There were good linear correlations between the concentrations and peak areas of the eight components with the correlation coefficients of 0.9982~0.9999. The average recoveries were 83.9 %~103.7 % with relative standard deviations of 1.6 %~4.6 % (n=5). The detection limits were 0.2~1.5 mg/L. The method of SPE-HPLC-PAD eliminated a great deal of interferences in wines effectively by optimizing extraction conditions.The eight biological activity were well separated and the analytical results were improved well and truly. The results for determining 7 market wines showed that as an important bioactive substance. the phenolic compounds content has close relationships with brewing methods, varieties of grape and producing areas.The results also showed that it is a convenient, rapid, sensitive and accurate method. It can be used to analyze these biological activity in other complex matrices.

Key words: solid phase extraction, HPLC-PAD, wines, phenolic compounds