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1、2009年3月色譜Vol.27No.2March2009ChineseJournalofChromatography244~247高速逆流色譜分離制備陳皮中的黃酮類化合物1113211孫印石,劉政波,王建華,王迎,祝麗香,李來玲(1.山東農(nóng)業(yè)大學(xué)農(nóng)學(xué)院,山東泰安271018;2.泰山林業(yè)科學(xué)研究院,山東泰安271000)摘要:應(yīng)用高速逆流色譜法分離制備了陳皮中3種黃酮類化合物。以石油醚2乙酸乙酯2甲醇2水(體積比為2∶4∶3∶3)為兩相溶劑系統(tǒng),在主機(jī)轉(zhuǎn)速850r/min、流動(dòng)相流速117mL/m
2、in、檢測波長280nm條件下進(jìn)行分離制備,6h內(nèi)從410g陳皮粗提物中一步分離制備得到橙皮苷1011mg、桔皮素4918mg和52羥基26,7,8,3′,4′2五甲氧基黃酮5016mg,純度均達(dá)9710%以上,各化合物結(jié)構(gòu)經(jīng)質(zhì)譜和核磁共振氫譜、碳譜鑒定。利用該方法可以對陳皮中的黃酮類化合物進(jìn)行快速的分離和純化。關(guān)鍵詞:高速逆流色譜;橙皮苷;桔皮素;52羥基26,7,8,3′,4′2五甲氧基黃酮;陳皮中圖分類號:O658文獻(xiàn)標(biāo)識碼:A文章編號:100028713(2009)0220244204欄目
3、類別:技術(shù)與應(yīng)用PreparativeisolationandpurificationofflavonesfromPericarpiumCitriReticulataebyhigh2speedcounter2currentchromatography1113211SUNYinshi,LIUZhengbo,WANGJianhua,WANGYing,ZHULixiang,LILailing(1.CollegeofAgronomy,ShandongAgriculturalUniversity,Taian
4、271018,China;2.TaishanAcademyofForestry,Taian271000,China)Abstract:Threeflavoneswereprepared,isolatedandpurifiedfromPericarpiumCitriReticu2lataebyhigh2speedcounter2currentchromatography(HSCCC).Atwo2phasesolventsystemcomposedoflightpetroleum2ethylaceta
5、te2methanol2water(2∶4∶3∶3,v/v/v/v)wasused.Within6hours,1011mgofheseridin,4918mgof5,6,7,8,4′2pentamethoxyflavoneand5016mgof52hydroxy26,7,8,3′,4′2pentamethoxyflavonewiththeirpuritiesover9710%wereobtainedfrom410gofthecrudeextractofPericarpiumCitriReticul
6、ataeinone2stepelutionundertheconditionsofaflowrateof1170mL/min,800r/minandthedetectionwavelengthof280nm.Theobtainedfractionswereanalyzedbyhighperformanceliquidchromatography(HPLC),and113identifiedbymassspectrometry(MS),H2nuclearmagneticresonance(NMR)a
7、ndC2NMR.TheresultsindicatethatHSCCCisapowerfultechniqueforthepurificationofflavonesfromCitrusreticulataBlanco.Keywords:high2speedcounter2currentchromatography(HSCCC);hesperidin;5,6,7,8,4′2pentamethoxyflavone;52hydroxy26,7,8,3′,4′2pentamethoxyflavone;P
8、ericarpiumCitriReticulatae陳皮(PericarpiumCitriReticulatae)為蕓香chromatography,簡稱HSCCC)是一種液2液分配色科植物橘CitrusreticulataeBlanco及其栽培變種譜技術(shù)。與其他色譜分離方法相比,HSCCC不用任[1]的干燥成熟果皮,具有理氣、燥濕、化痰等作用。何固體載體或支撐體作為固定相,樣品只是通過互橙皮苷(Hesperidin)是陳皮中含量較高的特征性成不混溶的兩相溶劑間分配的不同而在短時(shí)間