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作 者:朱丹[1] 何世玲[1] 范华均[1] 王李平[1] 娄欣欣[1] 万强[1] 臧林泉[1]
出 处:《分析测试学报》2013年第9期1075-1080,共6页Journal of Instrumental Analysis
基 金:国家"重大新药创制"科技重大专项(2011ZX09102-001-31);广东药学院师资队伍建设基金项目(52104109)
摘 要:以乙醇-硫酸铵双水相体系为萃取溶剂,采用聚焦微波辅助萃取法萃取农吉利中的牡荆素和异牡荆素,HPLC测定,建立了微波辅助双水相萃取(FMAATPE)/HPLC方法测定牡荆素和异牡荆素含量的分析方法。利用单因素试验和正交试验设计方法优化了乙醇质量分数、微波功率、料液比、萃取时间等萃取条件以及色谱分析条件。萃取优化条件为:双水相的组成:35%乙醇-16%硫酸铵,药材颗粒度:80目,料液比:1∶50,微波功率:140 W,萃取时间:20 min。以乙腈-0.5%磷酸(14∶86)为流动相在340 nm检测可较好地分离目标组分。将该方法用于农吉利药材中牡荆素和异牡荆素的萃取测定,可获得满意结果,其回收率为96.9%-103.8%,RSD为1.9%-2.6%。A new method for analysis of vitexin and isovitexin in Crotalaria sessiliflora L.was developed by focused microwave-assisted aqueous two-phase extraction(FMAATPE) coupled with high performance liquid chromatography(HPLC).The experimental factors,including ethanol concentration,ratio of material to solvent,microwave power and extraction time were optimized based on the single factor test and orthogonal test.The analysis was performed by HPLC with UV detection at 340 nm.The mobile phase consisted of acetonitrile-water containing 0.5% phosphoric acid(14∶86).The optimum extraction conditions were as follows:two-phase composition:35% ethanol-16% ammonium sulfate,ratio of material to solvent:1∶50,microwave power:140 W, extraction time:20 min.The method was applied in the determination of vitexin and isovitexin in Crotalaria sessiliflora L.,with recoveries of 96.9%-103.8% and RSDs of 1.9%-2.6%.
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