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时间:2020-04-20
《快速高效提取并检测银杏内酯的一种新方法.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、·336·实用医药杂志20l4年04月第31卷第04期PracJMed&Pha1311.Vol3l。2014—04No.04药学·论著·决速高效提取并检测银杏内酯的一种新方法六王琳,朱缨,吴纪凯[摘要]目的银杏叶是参银复智制剂的君药,寻找快速简便的方法从银杏叶中提取分离检测有效成分白果内酯和银杏内酯A、B、C。方法采用超高效液相色谱法(UPLC),色谱柱:watersBEHC18,2.1x50mm,1.7Ixm;流动相:甲醇一四氢呋喃一水(25:5:70);流速0.3ml/min;柱温:30℃;蒸发光散射检测器(EIJsD)。银杏叶采用7倍70%乙醇溶液回流提取2次,3h/次,合并提取液,减压
2、回收乙醇,加3倍量水使沉淀,过滤,滤液分别上大孔吸附树脂D101、AB一8、D201、聚酰胺树脂,考察洗脱剂的浓度和用量。结果选择聚酰胺树脂,2倍水洗后,用2—3倍树脂床体积l0%乙醇溶液洗脱,收集洗脱液,减压浓缩干燥,检测含量,银杏萜类内酯的含量都在35%以上,有效部位得率在90%以上。结论超高效液相色谱法简便快速、回收率高,为银杏叶中内酯类物质的提取分离检测提供了一种新方法。[关键词]银杏内酯;超高效液相色谱法;树脂分离;参银复智剂[中图分类号]R284[文献标识码]AAnewmethodtoextract,separateanddetectYinxingterpenelactonesfr
3、omGinkgobilobaleavesWANGLin,ZHUYin,WUJi-kai.SuzhouHealthOccupationPoly-technicCollege,Suzhou,Jiangsu215009,China[Abstract]0bjectiveToestablishasimpleandrapidmethodforextraction,separationanddetectionbilobalideandginkgolideA,B,andCfromGinkgobilobaleaves.MethodsUltraperformanceliquidchromatographwithe
4、vaporativelightscanningdetector(UPLC—ELSD)methodwasadopted:watersBEHCis(2.1x50mm,1.7tzm)column,mobilephase:methanol—tetrahydrofuran—water(25:5:70)ataflowrateof0.3ml/min,columntemperature30℃.ThedetectionwascarriedoutwithELSDdetector.TheGinkgobilobaleaveswasextractedwith7timesof70%ethanol,refluxedfor2
5、hourseachtime,theextractionsolutionwascombined,removedtheethanolundervacuum,added3timesofwatertoprecipitatetheimpurity,thefiltratewasthroughtheDlO1resincolumn,AB一8resincolumn,D201resincolumnandpolyamidecolumnrespectively.ResultsTheoptimizedconditionstoprepareYinxingterpenelactonesintheGinkgobilobale
6、avesfiltratewasthroughpolyamidecolumn,washedwith2timeswaterandthenelutedwith2—3BVof10%ethano1.thecollectedelutionofwaterandethanolwereconcentratedundervacuum.thentheYinxingterpenelactoneswereobtained.withtheconcentrationatmorethan35%andtheyieldrateatmorethan90%.ConclusionAbovemethodwhichissimpleandr
7、apidcanprovideanewwaytoextract,separateanddetectYinxingterpenelactonesfromGinkgobilobaleaves.[Keywords]Yinxingterpenelactones;UPLC(ultraperformanceliquidchromatography);Separationbyresin;Shenyinfuzhip
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