摘要
目的建立测定肺脾气虚汤中15个主成分(原儿茶醛、芒柄花素、芹菜素、刺槐素、甘草苷、异槲皮苷、去氢土莫酸、茯苓新酸A、橙皮苷、白术内酯Ⅲ、毛蕊异黄酮、桔皮素、川陈皮素、芒柄花苷、毛蕊异黄酮苷)含量的方法。方法采用超高效液相色谱串联质谱法(UHPLC-MS/MS),色谱柱为Agilent ZORBAX SB-C_(18)(2.1 mm×100 mm,3.5μm),流动相A为0.1%甲酸乙腈溶液,流动相B为0.1%甲酸-5 mmol/L醋酸铵溶液,梯度洗脱,流速0.4 ml/min,柱温35℃,以利血平为内标,采用正离子监测模式同时测定川陈皮素、桔皮素、白术内酯Ⅲ、毛蕊异黄酮苷、毛蕊异黄酮和芒柄花苷6种主成分含量;采用负离子监测模式同时测定甘草苷、橙皮苷、芒柄花素、茯苓新酸A、去氢土莫酸、刺槐素、芹菜素、异槲皮苷和原儿茶醛9种主成分含量。结果肺脾气虚汤中15种主成分的线性关系、重复性和精密度良好,平均回收率为95.53%~108.96%。结论该方法操作简便、灵敏度高、重复性好,为肺脾气虚汤的质量控制提供了实验室依据。
Objective To establish a method for the determination of 15 main components(i.e.protocatechuic aldehyde,formononetin,apigenin,acacetin,liquiritin,isoquercitrin,dehydrotumoic acid,poricoic acid A,hesperidin,atractylenolide Ⅲ,calycosin,tangeretin,nobiletin,ononin,and calycosin glycoside)in Feipiqixu decoction.Methods The method was developed using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)and the Agilent ZORBAX SB-C_(18)(2.1×100 mm,3.5μm)column was chosen for chromatographic separation with column temperature maintained at 35℃.The mobile phase consisted of A(0.1%formic acid acetonitrile solution)and B(0.1%formic acid-5 mmol/L ammonium acetate solution),and was delivered at 0.4 ml/min in gradient elution mode.The reserpine was utilized as an internal standard.Both positive and negative ionization modes were used successfully to detect the 6 main components(nobiletin,tangeretin,atractylenolide Ⅲ,calycosin glycoside,calycosin,ononin)and the 9 components(protocatechuic aldehyde,formononetin,apigenin,acacetin,liquiritin,isoquercitrin,dehydrotumoic acid,poricoic acid A,hesperidin)in Feipiqixu decoction.Results The linearity,repeatability and precision of the 15 principal components in Feipiqixu decoction were good,with an average recovery rate ranging from 95.53% to 108.96%.Conclusion The method is easy to operate with high sensitivity and good repeatability,and could provide laboratory basis for the quality control of Feipiqixu decoction.
作者
王贞丽
王志鹏
崔莉莉
宋新华
许封菁
高守红
Wang Zhenli;Wang Zhipeng;Cui Lili;Song Xinhua;Xu Fengjing;Gao Shouhong(Department of Quality Management,Navy Qingdao Special Service Convalescent Center,Qingdao 266071,China)
出处
《海军医学杂志》
2022年第8期841-846,共6页
Journal of Navy Medicine
关键词
新冠肺炎
肺脾气虚汤
超高效液相串联质谱
含量测定
质量控制
COVID-19
Feipiqixu decoction
Ultra-high performance liquid chromatography-tandem mass spectrometry
Content determination
Quality Control
