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作 者:李肖 刘洋洋 曹江营 毛蓓蓓 李克杰 赵东升 LI Xiao;LIU Yang-yang;CAO Jiang-ying;Mao Bei-bei;LI Ke-jie;ZHAO Dong-sheng(Shandong University of Traditional Chinese Medicine,Ji'nan 250355,China)
出 处:《时珍国医国药》2023年第8期1885-1888,共4页Lishizhen Medicine and Materia Medica Research
基 金:国家自然科学基金(82204656);山东省中医药科技发展计划项目(2019-0030);山东中医药大学中药资源保护与质量评价青创团队支持项目。
摘 要:目的建立同时测定产后逐瘀胶囊中10个成分含量的方法。方法采用Zorbax Eclipse Plus C18色谱柱(2.1 mm×100 mm,1.8μm)、流动相0.1%甲酸水-乙腈进行梯度洗脱,流速0.35 mL·min^(-1),柱温40℃;质谱为电喷雾离子源(ESI)、正负离子扫描的多反应监测模式(MRM)。结果益母草碱、水苏碱、咖啡酸、阿魏酸、洋川芎内酯I、洋川芎内酯H、6-姜辣素、洋川芎内酯A、藁本内酯和6-姜烯酚分别在22.56~1443.75、33.50~8575.00、7.13~456.25、10.94~700.00、14.06~450.00、12.89~412.50、10.06~643.75、15.53~993.75、17.38~1112.50和18.46~590.63 ng·mL^(-1)质量浓度范围内线性关系良好;精密度、重复性和稳定性RSD均小于5.91%;加样回收率在80.66%~108.37%,RSD在1.74%~5.98%。12批胶囊中益母草碱、水苏碱、咖啡酸、阿魏酸、洋川芎内酯I、洋川芎内酯H、6-姜辣素、洋川芎内酯A、藁本内酯和6-姜烯酚的含量分别在386.96~707.49、3988.18~8083.22、85.48~226.35、239.04~578.10、87.20~325.09、46.66~227.09、59.93~184.20、417.62~1039.34、573.74~1196.23和27.73~107.22μg·g^(-1)范围内。结论该方法准确、灵敏、可靠,可为产后逐瘀胶囊的质量控制提供一定参考。Objective To establish a method for simultaneous determination of 10 constituents in Chanhou Zhuyu capsules.Meth⁃ods The quantification was conducted on an Agilent Zorbax Eclipse Plus C18 column(2.1 mm×100 mm,1.8μm).The mo⁃bile phase was consisted of acetonitrile and 0.1%formic acid solution for gradient elution with the flow rate of 0.35 mL·min-1.The column temperature was kept at 40 C.And the compounds were analyzed by electrospray ionization source(ESI)using multi⁃ple reaction monitoring(MRM)in both positive and negative ion modes.Results Leonurine,stachydrine,caffeic acid,ferulic acid,senkyunolide I,senkyunolide H,6-gingerol,senkyunolide A,ligustilide and 6-shogaol showed good linearities in the range of 22.56~1443.75,33.50~8575.00,7.13~456.25,10.94~700.00,14.06~450.00,12.89~412.50,10.06~643.75,15.53~993.75,17.38~1112.50 and 18.46~590.63 ng·mL-1,respectively.The RSDs of the precision,repeat⁃ability and stability tests were below 5.91%.The recoveries were in the range of 80.66%~108.37%with the RSD between 1.74%and 5.89%.The contents of leonurine,stachydrine,caffeic acid,ferulic acid,senkyunolide I,senkyunolide H,6-gin⁃gerol,senkyunolide A,ligustilide and 6-shogaol in 12 batches of Chanhou Zhuyu capsules were 386.96~707.49,3988.18~8083.22,85.48~226.35,239.04~578.10,87.20~325.09,46.66~227.09,59.93~184.20,417.62~1039.34,573.74~1196.23 and 27.73~107.22μg·g-1.Conclusion The method is sensitive,stable and reliable,and can be provide a refer⁃ence for the quality control of Chanhou Zhuyu capsules.
关 键 词:产后逐瘀胶囊 超高效液相色谱串联质谱 同时测定 质量控制
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