高效液相色谱法同时测定石上柏中4个双黄酮类化合物  

Simultaneous determination of four biflavonoids in Selaginella doederleinii Hieron by HPLC

作　　者：黄建勇[1,2] 李少光[2] 赵美凤[2] 李宇翔[2] 林新华[2] 姚宏[2] 

机构地区：[1]福建医科大学附属协和医院药学部,福建福州350001 [2]福建医科大学药学院药物分析系,福建福州350004

出　　处：《中国医院药学杂志》2013年第23期1945-1948,共4页Chinese Journal of Hospital Pharmacy

基　　金：国家自然科学基金项目(No.81202987;21275028);福建省自然科学基金(2012J01131;2012J05134)

摘　　要：目的：建立同时测定石上柏中穗花杉双黄酮、罗伯斯特双黄酮、2′′, 3′′-二氢-3′, 3′′′-双芹菜素及3′, 3′′′-双柚皮素共4个主要双黄酮成分的含量分析方法，为石上柏药材抗癌药用提供质量控制方法参考。方法：采用Ultimate· XB-C18 （4.6 mm ×250 mm，5 μm）色谱柱；以不同浓度的乙腈（B）-0.5%醋酸溶液（A）为流动相，检测波长270 nm，流速1.0 mL·min-1，柱温30 ℃。结果：穗花杉双黄酮、罗伯斯特双黄酮、2′′, 3′′-二氢-3′, 3′′′-双芹菜素和3′, 3′′′-双柚皮素均在1.56～100 μg·mL-1范围内具有良好的线性关系（r≥0.9999），平均加样回收率分别为99.0%, 96.0% 101.0% and 97.0%，RSD均小于5% （n=6）。结论：该法简便、快速，重现性好，可为石上柏药材质量控制提供定量分析方法。OBJECTIVE To establish a HPLC method for simultaneous determination of four main biflavonoids including amentoflavone, robustflavone, 2″, 3″-dihydro 3″, 3″ biapigenin and 3″ ,3″-binaringenin in Selaginella doederleinii Hieron and to provide a methodological reference for the quality control of Selaginella doederleinii Hieron in its antitumor usage. METH- OIlS Chromatographic experiment was carried out on an Uhimate^TM XB-C18 colunm （250 mm× 4. 6 mm,5μm） with a gradient eIution composed of acetonitrile （B） and 0.2% acetic acid （A）. The flow rate was 1. 0mL·min^-1 and the detection wavelength was 270 nm. The column temperature was set at 30℃. RESULTS The calibration curve showed good linearity over the, ranges of 1.56- 100μg·mL^-1 for amentoflavone, robustflavone, 2″, 3″ dihydro-3＇, 3″-biapigenin and 3＇, 3″ binaringenin （r≥ 0. 999 9）, respectively. The average recovery for the four compounds was 99. 0%, 96. 0%, 101. 0% and 97.0%, respectively. with the corresponding RSDs below 5% （n = 6）. CONCLUSION This method is simple, rapid, and reproducible. It can be used as a quantitative analysis method for the quality control of Selaginella doederleinii Hieron.

关 键 词：石上柏 双黄酮类化合物 含量测定 高效液相色谱法 

分 类 号：R969.3[医药卫生—药理学]