建立了超高液相色谱-串联四级杆质谱联用(UPLC-MS/MS)技术同时检测樱桃酒中没食子酸、4-羟基苯甲酸、绿原酸、香草酸和咖啡酸5种生物活性酚酸的方法。采用Waters Acquity UPLC BEH色谱柱(100×2.1mm,1.7μm),流动相为甲醇-0.1%甲酸,在梯度条件下进行分析,分析物在负离子模式下用保留时间和质谱信息进行定性,峰面积进行定量,并评价其定量分析的精密度、线性和检出限。结果显示,回收率在82.3%~110.8%之间;相关系数r>0.99,线性关系良好;精密度的相对标准偏差RSD<2.0%,检出限为0.020~0.050mg/L,说明该方法简便、快速、准确、灵敏,可用于樱桃酒中酚酸的检测。此外,实验采用SPSS17.0软件对樱桃酒的理化指标和5种酚酸进行了简单相关分析。
A method was developed for the simultaneous determination of gallic acid,p-hydroxybenzoic acid,chlorogenic acid,vanillic acid,and caffeic acid in cherry wines by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).The analytes were separated using an Acquity UPLC BEH C18 column(100×2.1mm,1.7μm) utilizing a gradient elution profile and a mobile phase of 0.1% formic acid and methanol.The analytes were detected using an electro spray ionization tandem mass spectrometry with negative ion mode.The five analytes were identified by retention time and mass spectrometry and quantified by peak area.This method was validated by recovery,linearity,and limits of detection(LOD).The recoveries of 5 phenolic acid standards are found in the range of 82.3%~110.8%.The correlation coefficient r is higher than 0.99.The relative standard deviations(RSD) are less than 2.0% and the LOD is between 0.020 mg/L and 0.050 mg/L.The method is convenient,rapid,accurate and sensitive,and could be used for the content determination of phenolic acid compounds in cherry wines.In addition,we estimate correlation between the physiochemical indexes and phenolic acids of cherry wines by SPSS 17.0 program.