青钱柳醇提物中化学成分的UHPLC-Q-TOF/MS分析

Analysis of Chemical Constituents in Ethanol Extract of Cyclocarya paliurus Dried Leaves by UHPLC-Q-TOF/MS

目的:应用超高效液相色谱-四极杆串联飞行时间质谱法(UHPLC-Q-TOF/MS)对青钱柳醇提物进行快速定性分析。方法:色谱条件为Poroshell 120 EC-C18色谱柱(3.0 mm×100 mm,2.7μm),以0.1%甲酸水溶液(A)-乙腈(B)为流动相梯度洗脱(0~26 min,2%~18%B;26~60 min,18%~72%B;60~70 min,72%~100%B;70~71 min,100%~2%B;71~72 min,2%B),流速0.4 mL·min^(-1),进样量3μL;质谱条件为电喷雾离子源(ESI),检测范围m/z 50~1100,正、负离子模式采集。通过安捷伦MassHunter工作站对所采集的数据进行处理,根据各化合物的保留时间、质谱信息,并结合现有文献及质谱数据库信息对化合物进行鉴定和裂解规律解析。结果:在正、负离子模式下,分别鉴定了52、55个化学成分,其中,正离子模式鉴定黄酮类14个、三萜类3个、有机酸类15个及其他类20个,负离子模式下则鉴定黄酮类18个、三萜类9个、有机酸类18个及其他类10个;汇总正、负离子模式并去除共有化合物,最终推测鉴定化合物87个,包括黄酮类22个、有机酸类27个、三萜类11个及其他类27个。结论:UHPLC-Q-TOF/MS技术可快速解析青钱柳的化学成分,1-酮糖和18β-甘草次酸等与青钱柳降糖活性相关的成分首次在该药材中被鉴定,可为阐明青钱柳药效物质基础提供实验依据。

Objective:Chemical components in ethanol extract of Cyclocarya paliurus dried leaves were analyzed by ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UHPLC-Q-TOF/MS).Method:An Agilent Poroshell 120 EC-C18 column(3.0 mm×100 mm,2.7μm)was used with 0.1%formic acid aqueous solution(A)-acetonitrile(B)as the mobile phase for gradient elution(0-26 min,2%^(-1)8%B;26-60 min,18%-72%B;60-70 min,72%^(-1)00%B;70-71 min,100%-2%B;71-72 min,2%B),and the flow rate of 0.4 mL·min^(-1) and injection volume of 3μL.The electrospray ionization(ESI)was used in positive and negative modes,and detection range was m/z 50^(-1)100.The collected data were processed by Agilent MassHunter workstation.According to the retention time and MS information of each compound,combined with existing literature and MS database information,the compounds were identified and analyzed for the fragmentation rule.Result:A total of 52,55 components were identified in the positive and negative ion modes,respectively.Among them,14 flavonoids,3 triterpenoids,15 organic acids and 20 other compounds were identified under positive ion mode,while 18 flavonoids,9 triterpenoids,18 organic acids and 10 other compounds were identified under the negative ion mode.By summarizing the positive and negative ion modes and removing the common compounds,87 compounds were identified,including 22 flavonoids,27 organic acids,11 triterpenoids and 27 other compounds.Conclusion:UHPLC-Q-TOF/MS can be used to quickly analyze the chemical constituents in C.paliurus dried leaves.1-Kestose and 18β-glycyrrhetinic acid and other components related to hypoglycemic activity of this herb are identified for the first time,which can provide reference for clarifying the pharmacodynamic substance basis of C.paliurus dried leaves.