欢迎来到天天文库
浏览记录
ID:55397550
大小:359.39 KB
页数:5页
时间:2020-05-15
《花椒油素的纯化和鉴定.pdf》由会员上传分享,免费在线阅读,更多相关内容在行业资料-天天文库。
1、现代食品科技ModernFoodScienceandTechnology2015,Vo1.31,No.1花椒油素的纯化和鉴定孙克奎(黄山学院旅游学院,安徽黄山245021)摘要:研究了从花椒中提取制备高纯花椒油素的方案。采用同时蒸馏萃取(SDE煨取花椒油素,利用硅胶柱色谱分离得到粗品,经过重结晶纯化得高纯花椒油素,利用核磁共振R)和反相高效液相色谱(RP—HPLC)进行定性和定量分析。在SDE过程中,料水比为1:10,溶剂(无水乙醚)用量为60mL,提取时间为1.5h时,粗提物中花椒油素含量达47.26%。以洗脱液配比(乙酸乙酯:石油醚)为l:
2、15、径高比为1:12、样品与硅胶质量比(上样量)为1:40、洗脱液流速为4mL/min的硅胶柱分离得到花椒油素粗品(纯度81.79%),回收率达99.12%。最后通过重结晶获得高纯花椒油素(纯度98.23%),总回收率达90.63%,得率为0.88%。NMR分析证实晶体确为花椒油素。该方案可实现从化a4-椒中高回收地制取高纯花椒油素,为拓宽花椒的精深加工提供参考。关键词:花椒;花椒油素;高效液相色谱;同时蒸馏萃取;硅胶;重结晶;核磁共振文章篇号:1673—9078(2,015)1.137141DOI:10.13982~.mfst.1673-9
3、078.2015.1.025Purificati0nandIdentificati0n0fXanthoxylinSUNKe-kui(TourismCollege,HuangshanUniversity,Huangshan245021,China)Abstract:Theaimofhisworkwastostudyanapproachforthepreparationofhigh—purityxanthoxylinfromZanthoxylumbungeanumMaxim.Xanthoxylinwasextractedbysimultaneous
4、distillationextraction(SDE),crudexanthoxylinwasisolatedusingasilicagelcolumn,andhigh-purityxanthoxylinwasobtainedbyrecrystallization.Nuclearmagneticresonance(NMR)andreversedphasehighperformanceliquidchromatography(RP—HPLC)wereusedforqualitativeandquantitativeanalysis,respect
5、ively.DuringtheSDE,thefollowingconditionswereused:materialtowaterratiol:10;solventvolume60mL;extractiontime1.5h.RP-HPLCanalysisshowedthatthexanthoxylincontentinthecrudeextractWas47.26%.Cmdexanthoxylinwasisolatedusingasilicagelcolumnunderthefollowingconditions:eluentratio(eth
6、ylacetate:petroleumether)1:15;diametertoheightratio1:12;sampletosilicagelratio1:40;eluentrate4mL/min.Thepurityoftheisolatedxanthoxylinwas81.79%andtherecover),was99.12%.Finally,high-purityxanthoxylin(98.23%1wasobtainedbyrecrystallization;thetotalrecoverywas90.63%andtheyieldwa
7、s0.88%.NMRanalysisshowedthattheisolatedcrystalWasxanthoxylin.Thus.thisapproachcouldachievethepreparationofhigh-purityxanthoxylin,withhigh-recovery,fromtheleavesofZanthoxylumbungeanumandserveasareferenceforbroadeningthescopeofZanthoxylumbungeanumdeep—processing.Keywords:Zanth
8、oxylumbungeanumMaxim.;xanthoxylin;highperformanceliquidchromatography;simul
此文档下载收益归作者所有