天然产物研究与开发 ›› 2019, Vol. 31 ›› Issue (11): 2001-2006.doi: 10.16333/j.10016880.2019.11.021

• 开发研究 • 上一篇    下一篇

青蒿素工业提取废料丙酮层中猫眼草黄素等3种多甲氧基黄酮富集研究

李鑫1,王可轩1,李东辉1,陈靖2,3*   

  1. 1哈尔滨商业大学药学院,哈尔滨 150076;2扬州大学医学院 转化医学研究院;3江苏省中西医结合老年病防治重点实验室,扬州 225001
  • 出版日期:2019-11-28 发布日期:2019-12-16
  • 基金资助:

    国家自然科学基金地区基金(81560580,81760377);宁夏自然科学基金(NZ17056)

Purification of three polymethoxylated flavonoids from the acetone layer of waste in artemisinin industrial production

LI Xin1,WANG Kexuan1,LI Donghui1,CHEN Jing2,3*   

  1. 1College of Pharmacy,Harbin University of Commerce,Harbin 150076,China;2Institute of Translational Medicine,Medical College,Yangzhou University;3Jiangsu Key Laboratory of Integrated Traditional Chinese and Western Medicine for Prevention and Treatment of Senile Disease,Yangzhou University,Yangzhou 225001,China
  • Online:2019-11-28 Published:2019-12-16

摘要: 为从青蒿素工业生产废料丙酮层中富集纯化猫眼草黄素、蒿黄素、槲皮万寿菊素3种活性多甲氧基黄酮。取一定量丙酮层,氯仿溶解,取与丙酮层生产废料质量相等的HPD100大孔树脂拌样,挥干后上HPD100大孔树脂,60%、70%、80%、90% EtOH/H2O依次进行洗脱;以RP-HPLC-UV为目标化合物追踪方法,取含目标化合物的70%洗脱部分,上硅胶柱,以石油醚丙酮梯度洗脱,100∶13馏份有黄色结晶(1),100∶15馏份有黄色结晶(2),100∶20馏份有黄色结晶(3),经TLC、RP-HPLC-UV及1H NMR、13C NMR分析,确定为猫眼草黄素(1,3 000 mg)、蒿黄素(2,1 000 mg)、槲皮万寿菊素(3,500 mg),以上既为后续药效学研究提供原料,也为青蒿素工业废料循环利用奠定重要基础。

关键词: 猫眼草黄素, 蒿黄素, 槲皮万寿菊素, 青蒿素工业废料, 多甲氧基黄酮

Abstract: This paper aimed to purify three active polymethoxylated flavonoids including chrysosplenetin,artemetin,and quercetagetin-3,7,3′,4′-tetramethyl ether from the acetone layer of waste in artemisinin industrial production.Acetone layer containing the targeted chemicals was dissolved in chloroform and mixed with same amount of HPD100 macroporous resin.The dried sample was added into the blank macroporous resin and gradient elution by 60%,70%,80%,and 90% EtOH/H2O was used to obtain the fraction containing the targeted chemicals under the monitoring of RP-HPLC-UV method.The 70% eluate was then chosen to further be isolated in silica gel column.A gradient elution by petroleum etheracetone was employed to gain compound 1 (yellow crystal) from 100∶13 fraction,compound 2 (yellow crystal) from 100∶15 fraction,and compound 3 (yellow crystal) from 100∶20 fraction.TLC,RP-HPLC-UV,1H NMR,and 13C NMR analysis were used to elucidate the structures of the three compounds to be chrysosplenetin (1,3 000 mg),artemetin (2,1 000 mg),and quercetagetin-3,7,3′,4′-tetramethyl ether (3,500 mg).This work provides enough source materials for further pharmacological study and lays the important basis of cyclic utilization for artemisinin industrial wastes.

Key words: chrysosplenetin, artemetin, quercetagetin-3,7,3&prime, ,4&prime, -tetramethyl ether;artemisinin industrial wastes, polymethoxylated flavonoids

中图分类号: 

R932