UPLC-MS同时测定蒙药材蓝刺头中6个成分的含量

摘要

目的:建立超高效液相色谱-串联质谱法(UPLC-MS)同时测定蒙药材蓝刺头中绿原酸、1,5-二咖啡酰奎宁酸、3,5-二咖啡酰奎宁酸、4,5-二咖啡酰奎宁酸、芹菜素和芹菜素-7-O-葡萄糖苷含量的方法.方法:样品分析采用Agilent 6430液质联用仪;色谱柱为Agilent ZORBAX RRHD Ecilipse Plus-C18;流动相为0.1％甲酸水溶液-甲醇,梯度洗脱;离子源为电喷雾电离源(ESI);采用负离子多反应监测模式(MRM).结果:绿原酸、3,5-二咖啡酰奎宁酸、1,5-二咖啡酰奎宁酸、芹菜素-7-O-葡萄糖苷、4,5-二咖啡酰奎宁酸和芹菜素分别在1.25 ～40.00(r =0.999 0)、0.94 ～30.00(r =0.999 8)、0.94 ～30.00(r =0.999 8)、0.16 ～5.00(r-0.999 7)、0.16～5.00(r =0.999 9)、0.02 ～2.50(r =0.999 5)μg·mL-1线性关系良好;加样回收率为99.80％～102.97％,RSD为1.23％ ～ 2.98％.结论:该方法专属性强、精密度高、重复性好,为蒙药材蓝刺头的成分研究提供科学参考.%Objective:To develop a specific UPLC-MS method for the determination of chlorogenic acid,1,5-dicaffeoylquinic acid,3,5-dicaffeoylquinic acid,4,5-dicaffeoylquinic acid,apigenin,and apigenin-7-O-glucoside in the flowers of Echinops latifolius Tausch..Methods:By using the UPLC-MS method,the six compounds were separated on an Agilent ZORBAX RRHD Ecilipse Plus-C18 column with a mobile phase consisted of water containing 0.1％ formic acid and methanol with gradient elution.Electrospray ionization source was applied and operated in negative ionization multiple reaction monitoring model(MRM).Results:The linear ranges of chlorogenic acid,3,5-dicaffeoylquinic acid,1,5-dicaffeoylquinic acid,apigenin-7-O-glucoside,4,5-dicaffeoylquinic acid,and apigenin were 1.25-40.00 (r =0.999 0),0.94-30.00(r=0.9998),0.94-30.00(r=0.999 8),0.16-5.00(r=0.9997),0.16-5.00(r=0.9999),0.02-2.50(r=0.999 5) μg· mL-1,respectively.The recoveries of six analytes ranged from 99.80％ to 102.97％,and the relative standard deviations were in the range of 1.23％ to 2.68 ％.Conclusion:The method is sensitive,accuracy and suitable for the determination of main compounds in the flowers of E.latifolius.