摘要
目的建立超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap-MS)法同时测定夏枯草配方颗粒中奎宁酸、丹参素、原儿茶酸、原儿茶醛、咖啡酸、异迷迭香酸苷、迷迭香酸、新绿原酸、秦皮乙素、绿原酸、隐绿原酸、阿魏酸、水杨酸、异槲皮苷、金丝桃苷、芦丁的含量。方法分析采用ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm);流动相0.1%甲酸-甲醇,梯度洗脱;体积流量0.3 mL/min;柱温40℃;电喷雾离子源;正负离子扫描。再进行主成分分析、正交偏最小二乘判别分析。结果16种成分在各自范围内线性关系良好(R^(2)≥0.9977),平均加样回收率87.72%~111.52%,RSD 0.61%~11.99%。16批样品聚为4类,4个主成分累积方差贡献率为87.74%,丹参素、咖啡酸、异迷迭香酸苷、迷迭香酸、奎宁酸、金丝桃苷、芦丁、异槲皮苷、原儿茶醛、原儿茶酸为潜在质量标志物。结论该方法简便准确,稳定性好,可用于夏枯草饮片、配方颗粒的质量控制。
AIM To establish a ultra-performance liquid chromatography-quadrupole-electrostatic field orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap-MS)method for the simultaneous content determination of quinic acid,danshensu,protocatechuic acid,protocatechualdehyde,caffeic acid,salviaflaside,rosmarinic acid,neochlorogenic acid,esculetin,chlorogenic acid,cryptochlorogenic acid,ferulic acid,salicylic acid,isoquercitrin,hyperoside and rutin in Xiakucao Formula Granules.METHODS The analysis was performed on a 40℃ thermostatic ACQUITY UPLC BEH C_(18)column(2.1 mm×100 mm,1.7μm),with the mobile phase comprising of 0.1%formic acid-methanol flowing at 0.3 mL/min in a gradient elution manner,and electron spray ionization source was adopted in positive and negative ion scanning.Subsequently,principal component analysis and orthogonal partial least squares discriminant analysis were performd.RESULTS Sixteen constituents showed good linear relationships within their own ranges(R^(2)≥0.9977),whose average recoveries were 87.72%-111.52%with the RSDs of 0.61%-11.99%.Sixteen batches of samples were clustered into 4 types,4 principal components demonstrated the accumulative variance contribution rate of 87.74%,danshensu,caffeic acid,salviaflaside,rosmarinic acid,quinic acid,hyperoside,rutin,isoquercitrin,protocatechualdehyde and protocatechuic acid were taken as potential quality markers.CONCLUSION This simple,accurate and stable method can be used for the quality control of decoction pieces and formula granules of Prunella vulgaris L..
作者
华杰凯
张灿
沈杰
庄俊嵘
王琴
常昕楠
刘伟
张建伟
HUA Jie-kai;ZHANG Can;SHEN Jie;ZHUANG Jun-rong;WANG Qin;CHANG Xin-nan;LIU Wei;ZHANG Jian-wei(National Administration of Traditional Chinese Medicine Third Grade Laboratory for Traditional Chinese Preparations,Department of Pharmacy,Shuguang Hospital Affiliated to Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;School of Pharmacy,Hangzhou Normal University,Hangzhou 311121,China)
出处
《中成药》
北大核心
2026年第1期9-17,共9页
Chinese Traditional Patent Medicine
基金
中国科协青年托举工程项目(2020QNRC001)
上海中医药大学附属曙光医院信息化建设专项(SGYYXX-201905)。
关键词
夏枯草配方颗粒
化学成分
含量测定
超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap-MS)
主成分分析
正交偏最小二乘判别分析
Xiakucao Formula Granules
chemical constituents
content determination
ultra-performance liquid chromatography-quadrupole-electrostatic field orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap-MS)
principal component analysis
orthogonal partial least squares discriminant analysis
