白藓皮中活性物质梣酮的提取工艺研究

Extraction Techniques of Fraxinellone with Bioactivity from Dictamnus dasycarpus Turks

梣酮是白藓皮中具有生物活性的物质。采用ρ〔Ca(OH)2〕=100 g/L的石灰乳润湿药材,石油醚回流提取,浸膏用甲醇和石油醚分离,甲醇重结晶;V(环己烷)∶V(乙酸乙酯)=3∶2作洗脱剂,柱色谱进一步纯化,得无色针状结晶;经HPLC1、HNMR和13CNMR检测为梣酮。由该工艺获得的梣酮收率达到94.7%,且经小叶碟添加法活性测试证实,具有较高的生物活性,在w(梣酮)=0.21%时,其72 h的拒食率和死亡率分别为90.4%和95.2%。该提取分离工艺已于2008年1月24日申请中华人民共和国国家发明专利"梣酮的新用途及梣酮水剂杀虫剂"(申请号200810017515.7)。

In order to extract the fraxinellone with bioactivity containing in Dictamnus dasyearpus Turks, 100 g/L milk of lime wetting plant material, was extracted by using refluent extract method with petroleum ether as a solvent. The residue was separated with methanol and petroleum ether, and recrystallized in methanol. It was further purified on a silica gel column using cyclohexane/ethyl acetate （3：2 by volume） as eluent. The colorless needles were identified as fraxinellone by HPLC, ^1HNMR and ^13CNMR. The yield of fraxinellone was 94.7% using this simple technique. The product exhibited a better biological activity by the bioassays using the leaf disk method. Its antifeeding rate and death rate of 72 h at 0. 21% （ mass percent） against Mythimna setarata were 90. 4% and 95.2%, respectively. This work has been applied to a National Invention Patent of China on Jan. 24,2008 ,＂a new purpose of fraxinellone and its water solubility pesticide＂ （ No. 200810017515. 7 ）.