超高效液相色谱串联质谱法测定葡萄酒中酚酸和酚醛类化合物

Determination of Phenolic Acids and Phenol Aldehyde Compounds in Wine by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

建立了超高效液相色谱-三重四极杆串联质谱法检测葡萄酒中18种酚酸和酚醛类物质的方法。将葡萄酒经0.22μm PTFE滤膜过滤后进样,选用ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm),以0.1%(V/V)甲酸乙腈溶液-0.1%(V/V)甲酸水溶液为流动相,采用梯度洗脱方式,对酚类物质进行分离。选择电喷雾离子源(ESI),采用多反应监测(MRM)的模式,优化质谱参数。实验结果表明,18种酚酸和酚醛类物质在各自的质量浓度范围内均呈良好的线性关系,检出限在0.2~4μg/L之间,定量限在0.8~10μg/L之间,平均回收率为75.0%~98.8%,精密度为1.68%~6.19%。利用上述方法对葡萄酒样品进行分析,结果表明,所有葡萄酒中均含有没食子酸、咖啡酰酒石酸、对羟基苯甲酸、丁香酸、香草酸等酚类物质,未检出原儿茶酸、鞣花酸、水杨酸和肉桂酸等,部分酒样中检出芥子酸。该方法能够满足葡萄酒酚酸和酚醛类物质检测的定量和定性要求。

A method for the separation of 18 kinds of phenolic acid and phenol aldehyde compounds in wine was developed by ultra performance liquid chromatography tandem mass spectrometry.Wines filtered after 0.22μm membrane were analyzed using ACQUITY UPLC HSS T3(2.1 mm×100 mm,1.8μm).The composition were isolated by the mobile phase of 0.1%(V/V)formic acid acetonitrile and 0.1%(V/V)formic acid water using gradient elution.The qualitative and quantitative analyses were operated under multiple reaction monitoring(MRM)mode using electrospray ion source(ESI)mode.The test results showed that the compounds to be tested presented a good linear relationship in respective mass concentration ranges.The limits of detection(LODs)were between 0.2~4μg/L and the limits of quantification(LOQs)were 0.8~10μg/L.The average recovery was in the range of 75.0%~98.8%with the precision from 1.68%to 6.19%.The above methods were used to analyze the wine samples.The results showed that gallic acid,caftaric acid,p-hydroxybenzoic acid,syringic acid,vanillic acid and other phenolic substances were found in all wines.Ellagic acid,3,4-dihydroxybenzoic acid,salicylic acid and cinnamic acid were not detected in wine.Sinapic acid was detected in a few wine samples.This method was proved to be accurate for the analysis of phenolic acid and phenol aldehyde compounds in wine.