土木香内酯与异土木香内酯的提取与纯化工艺_英文_张乐

27:126-133天然产物研究与开发NatProdResDev2015,

6880(2015)1-0126-08文章编号:1001-

土木香内酯与异土木香内酯的提取与纯化工艺

张乐,王梦月,李晓波

*

上海交通大学药学院中药基因组学实验室,上海200240

要:本文报道了一种从土木香药材中提取以及纯化倍半萜内酯的方法。乙醇回流提取的方法采用正交试

L9(34)],验设计方法[考察了4个因素对产率与内酯浓度的影响,最终确定了乙醇回流提取的最佳方法:药材2h。而硅胶柱层析的最佳纯化方法为:以100~200目的硅胶,1∶3加热回流提取1次,加10倍量的95%乙醇,

v/v),的上样量,径高比为1∶2。其洗脱剂成分为石油醚∶丙酮(100∶3,洗脱流速为35mL/min。采用该方法,异土木香内酯与土木香内酯的提取率大于70%,其纯度大于90%。关键词:土木香内酯;异土木香内酯;正交试验;硅胶柱层析;土木香中图分类号:R932

文献标识码:A

DOI:10.16333/j.1001-6880.2015.01.026

ExtractionandPurificationofAlantolactoneand

IsoalantolcatonefromRootofInulahelenium

ZHANGLe,WANGMeng-yue,LIXiao-bo*

SchoolofPharmacy,ShanghaiJiaoTongUniversity,Shanghai200240,China

Abstract:TheextractionandpurificationmethodofsesquiterpenelactonesfromtherootofInulaheleniumL.wasopti-mized.Thetestsoforthogonalarraydesign[L9(34)]wereperformedtoanalyzetheeffectofsinglefactors,namelyetha-nolconcentration,extractiondurationandtimesofextraction,ontheextractionyieldofisoalantolcatoneandalantolac-tone.Astheresult,theoptimalextractionconditionswerefoundasfollows:thedriedrootsofI.heleniumwereextractedbyrefluxwith95%ethanolinsolid/liquidratioof1∶10(w/v)for2hrs.Theoptimizedpurificationprocessofethanolextractwasachievedbyapressurizedsilicagel(100-200mesh)columnchromatographywithdiametertoheightratioof1∶2.Theratioofmixedsampletosilicagelwas1∶3(w/w),theeluentcomposedofpetroleumether(30-60℃)andacetone(100∶3,v/v),flowedattherateof35mL/min.Theextractionyieldofthelactonesundertheoptimalmethodwasabove70%,andthepuritywasabove90%.

Keywords:Isoalantolcatone;alantolactone;orthogonalarraydesign;silicagelcolumnchromatography;InulaheleniumL.

Introduction

InulaheleniumL.(Compositae)isaperennialplant,distributedinmanyareasofChina,EuropeandNorthAmerica.TherootofI.heleniumisrichineudesmane-typesesquiterpenelactones,suchasisoalantolcatoneandalantolactone[1].Inrecentyears,extensiveinvesti-gationsonactiveconstituentsofI.heleniumrootsprovedthatsesquiterpenelactoneswereresponsibleforvariousbiologicalactivities,suchasantibacterial,anti-fungal,hepatoprotectiveandantitumoractivities[2-4].

Received:January20,2014Accepted:May7,2014

Foundationitem:MajorProgressofNationalNewDrugResearch(2012ZX09103201-038)

*CorrespondingauthorTel:86-21-34204806;E-mail:xbli@sjtu.edu.cn

Therefore,itisnecessarytofindanefficientmethodforextractionandpurificationofsesquiterpenelactones.Thecurrentstudywasmainlyfocusedontheultrasonic-assistedextractionofphenolicandmicrowave-assisted

6]extractionofflavones[5,,butthepuritywasnotrepor-

ted.Inthisstudy,wereportanimprovedextractionmethodforsesquiterpenelactonesbyethanol-refluxandpurificationbysilicagelcolumnchromatography.Theextractionyieldofthelactonesobtainedbytheoptimalmethodwasabove70%,andthepuritywasabove90%.

Materialsandmethods

Plantmaterialandreagents

DriedrootsofI.heleniumwerepurchasedfromthe

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