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.