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作 者:李林[1] 关洪月[1] 殷放宙[1] 陆兔林[1] 林家红 蔡宝昌[1]
机构地区:[1]南京中医药大学国家教育部中药炮制规范化及标准化工程研究中心,南京210029 [2]南京海辰药业有限公司,南京210046
出 处:《中国实验方剂学杂志》2013年第24期66-70,共5页Chinese Journal of Experimental Traditional Medical Formulae
基 金:国家科技部重大专项(2009ZX09308-004);江苏高校优势学科建设工程项目(2011zyx2-009)
摘 要:目的:建立HPLC-MS同时测定芫花中木犀草素、芹菜素、羟基芫花素、芫花素以及芫花酯甲5种化学成分含量的方法,分析炮制前后含量的变化。方法:采用液质联用法,质谱采用大气压电喷雾离子源,选择性负离子模式监测。色谱柱为Agilent Zorbax C18(2.1 mm×50 mm,1.8μm),流动相为0.05%甲酸乙腈(A)-0.05%甲酸水(B),流速0.6 mL·min-1,柱温30℃,进样量2μL。结果:芫花炮制后5种毒效成分均发生了一定程度的变化。3种黄酮类有效成分木犀草素、羟基芫花素以及芫花素炮制后含量升高,二萜原酸酯甲代表成分芫花酯甲炮制后含量降低,黄酮类成分芹菜素经炮制后含量也发生了下降。结论:该方法简单、灵敏、准确,为芫花及其炮制品的质量评价提供了有效的方法。Objective: To establish a HPLC-MS method for the simultaneous quantitation of luteolin, apigenin, 3'-hydroxy-genkwanin, genkwanin and yuanhuacine in Genkwa Flos, and to analyze the content change before and after processing. Method: HPLC-MS was used for quantification in negative ion mode under ESI. Chromatography was performed on Agilent Zorbax C18(2.1 mm×50 mm, 1.8 μm) column by gradient elution using 0.05% formic acid in acetonitrile-0.05% formic acid in water at the flow rate of 0.6 mL·min-1. The column temperature was kept at 30℃ and the inject volume was 2 μL. Result: The content of five toxic and active compounds was all changed after processed. The content of the luteolin, 3'-hydroxy-genkwanin, genkwanin was higher and the apigenin and yuanhuacine were lower than the raw ones. Conclusion: The new developed LC-MS method is simple, sensitive and accurate. It can be used for the quality evaluation of crude and processed Genkwa Flos.
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