食品科学 ›› 2022, Vol. 43 ›› Issue (12): 252-254.doi: 10.7506/spkx1002-6630-20210731-380

• 成分分析 • 上一篇    

基于气相色谱-三重四极杆质谱联用法测定葡萄果实与葡萄酒中挥发性酚

杨薇熹,张思奇,向小凤,石英,段长青,兰义宾   

  1. (中国农业大学食品科学与营养工程学院,葡萄与葡萄酒研究中心,农业农村部葡萄酒加工重点实验室,北京 100083)
  • 发布日期:2022-07-01
  • 基金资助:
    北京市自然科学基金面上项目(6222035)

Determination of Volatile Phenols in Grape and Wine by Gas Chromatography-Triple Quadrupole Mass Spectrometry

YANG Weixi, ZHANG Siqi, XIANG Xiaofeng, SHI Ying, DUAN Changqing, LAN Yibin   

  1. (Key Laboratory of Viticulture and Enology, Ministry of Agriculture and Rural Affairs, Center for Viticulture and Enology, College of Food Science and Nutritional Engineering, China Agricultural University, Beijing 100083, China)
  • Published:2022-07-01

摘要: 利用固相萃取结合气相色谱-三重四极杆质谱联用技术,建立测定葡萄与葡萄酒中19 种挥发性酚的多反应监测方法。该方法分别在葡萄汁与葡萄酒2 种基质中验证,方法检出限为0.02~1.01 μg/L,定量限为0.08~3.36 μg/L,具有较广线性范围且R2大于0.99,加标回收率在81.99%~122.72%范围内。具有较高的灵敏度、准确性和精密度。该方法应用于10 个葡萄果实样品和10 款葡萄酒中挥发性酚的检测,在所有样品中均能检测到19 种挥发性酚,其中香草酸、香草醛和4-乙烯基苯酚是葡萄果实含量较高的3 种挥发性酚;4-乙基苯酚、3-乙基苯酚和4-乙烯基苯酚是葡萄酒中含量较高的3 种挥发性酚。所测样品中目标物质含量范围均在方法线性范围内,该方法具有普遍适用性。

关键词: 葡萄果实;葡萄酒;挥发性酚;固相萃取;气相色谱-三重四极杆串联质谱;多反应监测

Abstract: A method for the simultaneous determination of 19 volatile phenols in grape and wine was developed by solid phase extraction (SPE) combined with gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS/MS) operated in the multi-reaction monitoring (MRM) mode and was validated on grape juice and wine. The limits of detection and quantification of the developed method were found to be 0.02–1.01 μg/L and 0.08–3.36 μg/L, respectively. The method had a wide linear range with a correlation coefficient (R2) greater than 0.99. The recoveries of standard addition were in the range of 81.99%–122.72%. The method was proved to be highly sensitive, accurate and precise. Furthermore, this method was successfully applied to investigate the concentrations of volatile phenols in 10 grape samples and 10 wine samples. A total of 19 volatile phenols were detected in each of the 20 samples. The major volatile phenols in grape were vanillic acid, vanilaldehyde and 4-vinylphenol, while 4-ethylphenol, 3-ethylphenol and 4-vinylphenol were the major volatile phenols in wine. The content of volatile phenols in the measured samples was within the linear range of the method, indicating the universal applicability of this method.

Key words: grape; wine; volatile phenol; solid phase extraction; gas chromatography-triple quadrupole mass spectrometry; multiple reaction monitoring

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