逆流萃取法提取甘肃棘豆中的苦马豆素

以甘肃棘豆为原料,采用φ(CH3CH2OH)=75%的乙醇为溶剂回流提取,提取液回收乙醇后用浓度为2mol/L的盐酸调节pH至3~4。离心,取上清液用氯仿以40 mL/m in流速逆流萃取,除去小极性杂质。再用浓度为2 mol/L的氢氧化钠水溶液调pH至9~10,用正丁醇以40 mL/m in流速逆流萃取。萃取液回收正丁醇后上硅胶柱分离,氯仿-甲醇-氨水洗脱,并用甲醇-氯仿重结晶得白色针状结晶,经MS和NMR鉴定确定其化学结构为苦马豆素,提取率为23 mg/kg。

Counter-flow Extraction of Swainsonine from Oxytrops kansuensis

Oxytrops kansuensis was extracted using a solution of ethanol/water(75∶25,V/V) by countercurrent extraction under reflux.Ethanol in the extraction solution was reclaimed,and the solution was then adjusted to pH=3～4 with 2 mol/L hydrochloric acid and subsequently centrifugated.In order to remove impurity of small polarity,the supernatant solution was extracted with chloroform by counter-flow extraction(flow velocity 40 mL/min).Afterward,the aqueous phase was adjusted to pH=9～10 with 2 mol/L sodium hydroxide and then extracted with butanol by counter-flow extraction(flow velocity 40 mL/min).Then the butanol phase was isolated by silica gel columniation chromatogram with chloroform-methanol-ammonia liquor as eluant.The extract was purified by methanol-chloroform.Final product was a white needle crystal that was identified as swainsonine by means of MS and NMR.The yield of swainsonine was 23 mg/kg.