UPLC-MRM-MS法测定头花蓼药材中7个指标成分

Determination of Seven Components in Polygonum capitatum by UPLC-MRM-MS

建立头花蓼药材中没食子酸、原儿茶酸、陆地棉苷、槲皮苷、儿茶素、槲皮素-3-O-（2″-没食子酰基）-鼠李糖苷及槲皮素的UPLC-MRM-MS检测方法。色谱采用Waters BEH C18（2.1 mm×50 mm,1.7μm）色谱柱,以0.1%甲酸乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,质谱采用多反应离子监测（MRM）检测。没食子酸、原儿茶酸、陆地棉苷、槲皮苷、儿茶素、槲皮素-3-O-（2″-没食子酰基）-鼠李糖苷及槲皮素分别在0.136~32.965、0.031~7.481、0.022~5.300、0.076~18.433、0.085~20.737、0.017~4.147、0.128~31.029μg/m L浓度范围线性关系良好,平均回收率为91.23%~105.33%,RSD〈3%,精密度、重复性和稳定性良好。此方法操作简便,快速,灵敏度高,可用于头花蓼药材中主要活性成分的含量测定,并为头花蓼药材质量控制提供了新方法。

To establish a UPLC-MRM-MS method for the determination of gallic acid,protocatechuic acid,que-3-O-β-DGlc,quercitrin,catechin,que-3-O-（2″-O-galloyl）-β-D-Glc and quercetin in Polygonum capitatum. The analysis was achieved by BEH C18 column with a mobile phase composed of 0. 1% formic acid in acetonitrile and 0. 1% formic acid in water using gradient elution. A TQD tandem mass spectrometry was used as detector and operated by multiple reaction monitoring（MRM） mode. Good linearity was achieved for these components in the range of 0. 136-32. 965,0. 031-7.481,0. 022-5. 300,0. 076-18. 433,0. 085-20. 737,0. 017-4. 147,0. 128-31. 029 μg/m L,respectively. The average recoveries were 91. 23%-105. 33%,with RSD less than 3%. Precision,repeatability and stability were good. The developed method was simple,rapid,sensitive and suitable for the determination of the main active constituents in P. capitatum. It provided a new method for the quality control of P. capitatum.