摘要
目的 建立UPLC-MS/MS法同时测定六神曲中苦杏仁苷、咖啡酸、1,3-O-二咖啡酰奎宁酸、甲基原儿茶酸、伞形花内酯、东莨菪内酯、阿魏酸、牡荆素、金丝桃苷、异槲皮素、异绿原酸B、异绿原酸A、异绿原酸C、木犀草素C、槲皮素、芹菜素、异鼠李素、猫眼草酚D、异泽兰黄素、金腰乙素、蔓荆子黄素、滨蒿内酯、青蒿素B、洋艾素的含量.方法 分析采用Brownlee SPP C18色谱柱(2.1 mm×100 mm,2.7μm);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0.3 mL/min;柱温35℃;电喷雾离子源;正负离子扫描;多反应监测模式.再进行层次聚类分析、正交偏最小二乘判别分析,筛选差异成分.结果 24种成分在各自范围内线性关系良好(R2>0.9500),平均加样回收率95.06％～102.41％,RSD 0.90％～2.67％,不同批次样品中其含量差异明显.成都、杭州企业样品可被区分开,苦杏仁苷、阿魏酸、异槲皮素、槲皮素、青蒿素B是主要差异成分.结论 该方法快速灵敏,可为六神曲质量控制提供参考.
Abstract
AIM To establish a UPLC-MS/MS method for the simultaneous content determination of amygdalin,caffeic acid,1,3-O-dicaffeoylquinic acid,methyl protocatechuic acid,7-hydroxycoumarine,scopoletin,ferulic acid,vitexin,hyperoside,isoquercetin,isochlorogenic acid B,isochlorogenic acid A,isochlorogenic acid C,luteolin,quercetin,apigenin,isorhamnetin,chrysosplenol D,eupatilin,chrysosplenetin,vitexicarpin,scoparone,arteannuin B and artemitin in Massa Medicata Fermentata.METHODS The analysis was performed on a 35℃ thermostatic Brownlee SPP C18column (2.1 mm×100 mm,2.7 μm),with the mobile phase comprising of water (containing 0.1％ formic acid,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,hierarchical cluster analysis and orthogonal partial least squares discriminant analysis were performed,along with the screening of differential constituents.RESULTS Twenty-four constituents showed good linear relationships within their own ranges (R2>0.9500),whose average recoveries were 95.06％-102.41％ with the RSDs of 0.90％-2.67％,and the contents in different batches of samples demonstrated obvious differences.The samples from enterprises in Chengdu and Hangzhou could be distinguished,amygdalin,ferulic acid,isoquercetin,quercetin and artemisinin B were taken as main differential constituents.CONCLUSION This rapid and sensitive method can provide reference for the quality control of Massa Medicata Fermentata.
维普
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