UPLC-MS/MS法同时测定青果丸中15种成分的含量OA
Simultaneous content determination of fifteen constituents in Qingguo Pills by UPLC-MS/MS
目的 建立UPLC-MS/MS法同时测定青果丸中没食子酸、绿原酸、隐绿原酸、木犀草苷、异绿原酸C、槲皮素、蝙蝠葛苏林碱、哈巴俄苷、木犀草素、黄芩素、甲基麦冬黄烷酮B、蝙蝠葛碱、芍药苷、黄芩苷、汉黄芩素的含量.方法 分析采用Brownlee SPP C18色谱柱(2.1 mm× 100 mm,2.7 μm);流动相水(含0.1%甲酸、5 mmol/L乙酸铵)-乙腈,梯度洗脱;体积流量0.3mL/min;柱温35 ℃;电喷雾离子源;正负离子扫描;多反应监测模式.再进行聚类分析、主成分分析、正交偏最小二乘判别分析.结果 15种成分在各自范围内线性关系良好(R2>0.998 8),平均加样回收率94.52%~106.39%,RSD 0.21%~3.94%.22批样品聚为4类,4个主成分累积方差贡献率为83.808%,主要差异成分为异绿原酸C、木犀草苷、没食子酸、绿原酸、隐绿原酸、甲基麦冬黄烷酮B、蝙蝠葛苏林碱.结论 该方法准确灵敏,可用于青果丸的质量评价.
AIM To establish a UPLC-MS/MS method for the simultaneous content determination of gallic acid,chlorogenic acid,cryptochlorogenic acid,luteoloside,isochlorogenic acid C,quercetin,daurisoline,harpagoside,luteolin,baicalein,methylophiopogonanone B,dauricine,paeoniflorin,baicalin and wogonin in Qingguo Pills.METHODS The analysis was performed on a 35 ℃ thermostatic Brownlee SPP C18 column(2.1 mm×100 mm,2.7 μm),with the mobile phase comprising of water(containing 0.1%formic acid and 5 mmol/L ammonium acetate)-acetonitrile flowing at 0.3 mL/min in a gradient elution manner,and electron spray ionization source was adopted in positive and negative ion scanning with multiple reaction monitoring mode.Subsequently,cluster analysis,principal component analysis and orthogonal partial least squares discriminant analysis were performed.RESULTS Fifteen constituents showed good linear relationships within their own ranges(R2>0.998 8),whose average recoveries were 94.52%-106.39%with the RSDs of 0.21%-3.94%.Twenty-two batches of samples were clustered into four categories,four principal components demonstrated the accumulative variance contribution rate of 83.808%,isochlorogenic acid C,luteoloside,gallic acid,chlorogenic acid,cryptochlorogenic acid,methylophiopogonanone B and daurisoline were taken as differential components.CONCLUSION This accurate and sensitive method can be used for the quality evaluation of Qingguo Pills.
南丹慧;姚昱吏;康荣峰;马海棠;刘晓玲;李运;杨扶德
甘肃中医药大学药学院,甘肃兰州 730000甘肃中医药大学药学院,甘肃兰州 730000甘肃中医药大学药学院,甘肃兰州 730000甘肃中医药大学药学院,甘肃兰州 730000甘肃中医药大学药学院,甘肃兰州 730000兰州市食品药品检验检测研究院,甘肃兰州 730050甘肃中医药大学药学院,甘肃兰州 730000
医药卫生
青果丸化学成分含量测定UPLC-MS/MS聚类分析主成分分析正交偏最小二乘判别分析
Qingguo Pillschemical constituentscontent determinationUPLC-MS/MScluster analysisprincipal component analysisorthogonal partial least squares discriminant analysis
《中成药》 2026 (5)
1436-1443,8
国家药品监督管理局中药材及饮片质量控制重点实验室项目(2024GSMPA-KL)2021年度甘肃高等学校产业支撑计划项目(2021CYZC-40)兰州市人才创新创业项目(2023-RC-9)
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