色谱 ›› 2017, Vol. 35 ›› Issue (2): 178-184.DOI: 10.3724/SP.J.1123.2016.09009

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法检测红葡萄酒中功效成分

冯峰1, 程甲2, 粟有志3, 张峰1, 赵丹1   

  1. 1. 中国检验检疫科学研究院, 食品安全研究所, 北京 100176;
    2. 上海出入境检验检疫局动植物与食品 检验检疫技术中心, 上海 200135;
    3. 伊犁出入境检验检疫局综合技术服务中心, 新疆 伊宁 835000
  • 收稿日期:2016-09-02 出版日期:2017-02-08 发布日期:2013-06-09
  • 通讯作者: 张峰,E-mail:fengzhang@126.com
  • 基金资助:

    国家质检总局科技项目(2015IK311).

Determination of functional components in red wines by high performance liquid chromatography-tandem mass spectrometry

FENG Feng1, CHENG Jia2, SU Youzhi3, ZHANG Feng1, ZHAO Dan1   

  1. 1. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China;
    2. Technical Center for Animal Plant and Food of Shanghai Entry-Exit Inspection & Quarantine Bureau, Shanghai 200135, China;
    3. Comprehensive Technical Service Center of Yili Entry-Exit Inspection and Quarantine Bureau, Yining 835000, China
  • Received:2016-09-02 Online:2017-02-08 Published:2013-06-09
  • Supported by:

    Science and Technology Project of Administration of Quality Supervision, Inspection and Quarantine (AQSIQ) of China (No. 2015IK311).

摘要:

建立了高效液相色谱-串联质谱法快速测定葡萄酒中白藜芦醇、黄酮类、多酚类功效成分的分析方法。葡萄酒样品直接稀释后进样,用C18柱进行分离,以乙腈-0.1%(体积分数)甲酸水溶液为流动相进行梯度洗脱,通过多反应监测(MRM)模式进行检测。13种功效成分在各自线性范围内呈良好的线性关系,相关系数均大于0.99。除表没食子儿茶素、没食子儿茶素、儿茶素没食子酸酯、花旗松素的检出限为1.0、1.0、3.0、3.0 μg/L外,其他9种化合物的检出限均小于1.0 μg/L。回收率为80.9%~112.3%,相对标准偏差小于10%。该方法快速、准确、灵敏度高,适用于葡萄酒中功效成分的快速分析。对实际样品的检测表明,所测葡萄酒样品中均含有儿茶素、表儿茶素、表没食子儿茶素、没食子儿茶素、表儿茶素没食子酸酯/儿茶素没食子酸酯、白藜芦醇、大豆黄素等功效成分,不同品种葡萄酒中这些功效成分含量差异显著。

关键词: 串联质谱, 高效液相色谱, 功效成分, 红葡萄酒

Abstract:

A method for the determination of functional components in red wines by high performance liquid chromatography coupled with triple quadrupole mass spectrometry was developed. The wine samples were diluted 10 times directly and separated on a C18 column by gradient elution using acetonitrile-0.1% (v/v) formic acid aqueous solution as mobile phases. Electrospray ionization was applied and the qualitative and quantitative analyses were operated under multiple reaction monitoring (MRM) mode using positive and negative ion modes simultaniously. The calibration curves of 13 functional components showed good linearities (r>0.99) in their detection ranges. The limits of detection were less than 1.0 μg/L except for epigallocatechin (1.0 μg/L), gallocatechin (1.0 μg/L), catechin gallate (3.0 μg/L) and taxifolin hydrate (3.0 μg/L). The average recoveries ranged from 80.9% to 112.3%. The relative standard deviations were less than 10%. The method is quick, accurate, sensitive and suitable for the quantification of functional components in red wines. When the method was applied to commercial red wine samples, it was found that all selected wine samples contained catechin, epicatechin, epigallocatechin, gallocatechin, epicatechin gallate/catechin gallate, resveratrol, taxifolin hydrate, etc. In addition, the mass concentrations of functional components were significantly different among the red wines made from different species of grape.

Key words: functional components, high performance liquid chromatography (HPLC), red wines, tandem mass spectrometry

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