UPLC-MS同时测定蒙药材蓝刺头中6个成分的含量

Simultaneous Determination of Six Compounds in Echinops latifolius Tausch. Flowers by UPLC-MS

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-C_(18);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-Cls 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.