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高效液相色谱-电化学法测定四季青叶中4种化合物的含量

HPLC-ECD simultaneous determination of four compounds in leaves of Ilex purpurea Hassk.

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【作者】 潘娓婕刘琳刘晓星刘小莉郑建斌

【Author】 PAN Wei-jie School of Chemistry and Materials Science,Shaanxi Normal University,Xi’an 710062,China;LIU Lin LIU Xiao-xing LIU Xiao-li ZHENG Jian-bin Institute of Analytical Science,Northwest University/Shaanxi Province Key Laboratory of Electroanalytical Chemistry,Xi’an 710069,China)

【机构】 陕西师范大学化学与材料科学学院西北大学分析科学研究所/陕西省电分析化学重点实验室

【摘要】 目的:建立同时测定四季青叶中原儿茶酸、咖啡酸、槲皮素和山奈酚4种成分含量的高效液相色谱-电化学(HPLC-ECD)法。方法:采用 Zorbax SB-C18(150 mm×4.6 mm,5.0 μm)色谱柱;以(A)甲醇、(B)水-0.1%醋酸为流动相,梯度洗脱:0min 时 A-B(20:80),9 min 时 A-B(24:76),30 min 时 A-B(50:50),40 min 时 A-B(65:35);流速为0.8 mL·min-1,柱温为30℃,电化学检测器的工作电位为0.7 V,采用标准曲线法对4种化合物进行定量。结果:在选定的色谱条件下原儿茶酸、咖啡酸、槲皮素和山奈酚的检出限分别为3,6,2,5 ng,定量限分别为9.1,20.0,7.2,16.0 ng。4种化合物的平均加样回收率均在95.7%~102.6%之间,RSD 在1.6%~2.9%之间。结论:方法简便、准确,可用于同时检测四季青叶中4种化合物的含量。

【Abstract】 Objective:To establish an HPLC-ECD method for simultaneous determination of the contents of proto- catechuic acid,caffeic acid,quercetin and kaempferol in leaves of Ilex purpurea Hassk..Method:The separation was performed on Zorbax SB-C18column(150 mm×4.6 mm,5.0 μm)by gradient elution with(A)methanol- (B)water containing 0.1% acetic acid[0 min,A-B(20:80);9 min,A-B(24:76);30 min,A-B(50:50); 40 min,A-B(65:35)]as the mobile phase at a flow rate of 0.8 mL min-1.The detection was done at 0.7 V and 30℃.Calibration curves were applied to the determination of four compounds.Results:The limits of detection were 3 ng for protocatechuic acid,6 ng for caffeic acid,2 ng for quercetin and 5 ng for kaempferol and the limits of quan- tification were 9.1 ng for protocatechuic acid,20.0 ng for caffeic acid,7.2 ng for quercetin and 16.0 ng for kaempferol.The average recoveries of these compounds were between 95.7%-102.6% with RSDs of 1.6%- 2.9%.Conclusion:The method is simple,rapid,reproducible and accurate.It can be used for the routine analysis of the herb of Ilex purpurea Hassk..

【基金】 国家自然科学基金(批准号:20675062);陕西省自然科学基金(批准号:2004820);陕西省重点实验室访问学者项目(批准号:05JF17)
  • 【文献出处】 药物分析杂志 ,Chinese Journal of Pharmaceutical Analysis , 编辑部邮箱 ,2007年06期
  • 【分类号】R284
  • 【被引频次】4
  • 【下载频次】184
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