荨麻属植物大蝎子草化学成分及质量标准研究

Chemical Constituents and Quality Standard of Girardinia diversifolia(Link) Friis

目的研究荨麻属植物大蝎子草的化学成分及药材质量控制标准。方法采用硅胶柱色谱、薄层色谱等手段进行分离纯化,并通过波谱数据鉴定结构;采用TLC鉴别大蝎子草中东莨菪内酯,采用HPLC测定东莨菪内酯含量,以东莨菪内酯为对照,采用RP-HPLC,岛津-C18色谱柱(4.6 mm×250 mm,5μm),乙腈(A)-0.2%磷酸(B)梯度洗脱:洗脱程序0～5 min,A-B(25∶75)线性变化至A-B(20∶80);5～10 min,线性变化至A-B(15∶85);10～18 min,保持A-B(15∶85);18～19 min,A-B(50∶50);19～25 min,A-B(25∶75)。流速1 mL.min-1,检测波长298 nm,柱温30℃。结果分离鉴定了3个化合物,东莨菪内酯(1),山柰素(2),β-谷甾醇(3);定性鉴别薄层色谱特征明显,东莨菪内酯含量测定的线性范围为0.022～0.352μg(r=0.999 9),平均回收率(n=6)为92.93%(RSD 1.86%)。结论化合物东莨菪内酯、山柰素为首次从该植物中分离;建立的质量标准可准确地定性、定量,有效地控制大蝎子草药材的质量。

OBJECTIVE To study the chemical constituents and quality standard of Girardinia diversifolia （Link） Friis. METHODS The compounds were isolated by silica gel column chromatography and thin layer chromatography. Their structures were identified by physicochemical properties and various spectroscopic methods including NMR, MS, and UV, etc. Scopoletin in this prepa- ration was identified by TLC. Its content was determined by HPLC. The separation of scopoletin was performed on a Shimadzu C18 col- umn （4. 6 mm ×250 mm, 5 μm）. The mobile phase consisted of acetonitrile（A）-0. 2% phosphoric acid（B） ：0 -5 min,A-B（25：75） →A-B（20： 80） ;5 - 10 min,A-B（20： 80）→A-B（ 15： 85） ;10 - 18 min,A-B（ 15： 85） ;18 - 19 min,A-B（50： 50） ;19 -25 min,A-B （25： 75） ,with the flow rate of 1.0 mL · min-1 , the UV detection wavelength was 298 nm, and column temperature was 30 ℃. RE- SULTS Three compounds were isolated and identified as seopoletin （ 1 ）, kaempferol （2）, and/3-sitosterol. They showed obvious characteristics in TLC identification. Good linearity was obtained over the range of 0. 022 -0. 352 μg （r = 0. 999 9） for seopoletin. The average recovery （n = 6） was 92. 93 % （ RSD = 1.86% ）. CONCLUSION Compounds 1 -2 were isolated from the Girardinia diver- sifolia （Link） Friis for the first time. The qualitative and quantitative analysis methods are accurate and suitable for effective quality control of Girardinia diversifolia （Link） Friis.