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

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

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0.02~1.01μg/L,定量限为0.08~3.36μg/L,具有较广线性范围且R^(2)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。

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 0.02–1.01μg/L and 0.08–3.36μg/L,respectively.The method had a wide linear range with a correlation coefficient(R^(2))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.