13种多酚类异构体的超高效液相色谱-四级杆串联飞行时间质谱分析

Analysis of Thirteen Polyphenol Isomers by UPLC-QTOF Mass Spectrometry

建立了13种多酚类异构体的超高效液相色谱-四级杆串联飞行时间质谱(UPLC-QTOF-MS)分析方法。采用Kinetex 2.6μm Biphenyl色谱柱(2.1 mm×100 mm,100Å),以0.1%甲酸水溶液-甲醇/乙腈(V/V=30/70)为流动相,梯度洗脱,在负离子模式下全扫描采集;基于化合物一级精确质量数、同位素分布、二级全谱以及保留时间,对山奈酚、樱花素、绿原酸、橙皮甙及其异构体等13种多酚进行了分析。将建立的多酚类异构体筛查方法应用于桑叶茶和绿茶实际样品的分析,检测到绿原酸及其异构体和山奈酚-3-O-葡萄糖醛酸苷等7种组分。该方法可用于茶多酚等植物多酚类或有机合成多酚类化合物的快速筛查及定性定量分析。

An analysis method for thirteen polyphenol isomers by ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-QTOF-MS)was developed.Successful separation and detection of the isomers were achieved on a Kinetex 2.6μm Biphenyl column,in negative electrospray ionization mode.The mobile phase was 0.1%formic acid-methanol/acetonitrile(V/V=30/70)with gradient elution.The involved compounds include kaempferol,sakuranetin,chlorogenic acid,hesperidin and the corresponding isomers.The analysis was carried out by determining the retention times,accurate masses of quasi-molecular ions and their fragment ions,and isotopic patterns.The method was applied to real samples for screening of the involved polyphenols in mulberry leaf tea and green tea.The results showed that seven compounds were detected including chlorogenic acid and its isomers,and kaempferol-3-glucoside etc.This method is also applicable for rapid screening and accurate quantification of the described polyphenols in tea and other plant.