绿升麻中菠萝蜜烷型三萜类成分研究 2页

　　绿升麻中菠萝蜜烷型三萜类成分研究作者：卢滨范云双万定荣段宏泉【摘要】　　目的研究绿升麻中菠萝蜜烷型三萜皂苷类化学成分。方法以硅胶柱层析、凝胶层析等多种柱层析分离，制备高效液相色谱纯化，得到单体化合物，以各种有机波谱鉴定化合物结构。结果分离得到15个菠萝蜜烷型三萜类皂苷化合物，鉴定为asiaticosideA(1)；asiaticosideB(2)；26-deoxycimicifugoside(3)；cimicifugoside(23S,4)；25-甲氧基升麻醇-3-O-b-D-木糖苷(25-O-methyl-cimigenol-3-O-b-D-xylopyranoside,5)；25,2′-二乙酰升麻醇-3-O-β-D-木糖苷(25,2′-O-diacetylcimigenol-3-O-β-D-xylopyranoside,6)；24-乙酰升麻醇-3-O-β-D-木糖苷(24-O-acetylshengmanol-3-O-β-D-xylopyranoside(23R,24R,7)；24-O-acetyldahurinol-3-O-β-D-xylopyranoside(8)；23-乙酰升麻醇-3-O-β-D-木糖苷(23-O-acetylshengmanol-3-O-β-D-xylopyranoside,9)；CimiracemosideM(10)；12β-acetoxy-3β-hydroxy-24,25,26,27-tetranor-cycloart-7-en-23,16β-olide-3-O-β-D-xylopyranoide(11)；12β-acetoxy-3β-hydroxy-24,25,26,27-tetranor-cycloartan-23,16β-olide-3-O-β-D-xylopyranoide(12)；CimiracemosideH（13）；NeocimicigenosidesB(14)；2′-O-乙酰基-25-脱水升麻醇-3-O-β-D-木糖苷(2′-O-acetyl-25-anhydrocimigenol-3-O-β-D-xylopyranoside,15)。结论菠萝蜜烷型三萜类皂苷化合物3～15均为首次从绿升麻中分离得到。【关键词】绿升麻；醋酸乙酯提取物；菠萝蜜烷型三萜皂苷　　Abstract：ObjectiveToisolateandelucidatetheconstituentsofActaeaasiatiea.MethodsChemicalconstituentsnchromatography(ToyopearlH,12β-acetoxy-3β-hydroxy-24,25,26,27-tetranor-cycloart-7-en-23,16β-olide-3-O-β-D-xylopyranoside,12β-acetoxy-3β-hydroxy-24,25,26,27-tetranor-cycloartan-23,16β-olide-3-O-β-D-xylopyranoside,CimiracemosideH,NeocimicigenosidesB,2′-O-acetyl-25-anhydrocimigenol-3-O-β-D-xylopyranoside.Conclusionpound3～15Actaeaasiatiea.　　Keyent（TMS内标）;制备高效液相色谱仪：日本分光公司（JASCO）,PU-1580(泵),RI-1530和UV-1575（检测器）；制备色谱柱：YMC-PackODS-ASH-343-520X250mm（YMC），Econospheresilica10μm22X250mm(Alltech);液质联用色谱仪：Alliance2695,QuattroMicroTMESI(Sm/z:667［M+Na］+(分子式C37H56O9)。1H-NMR(300MHz,Pyr)δ:0.21,0.62(each1H,d,J=4.0Hz,19-H),0.91,1.04,1.14，1.17，1.19，1.24,1.30(each3H, s，7×CH3),2.15(3H,s,COCH3),4.82(2H,d,J=2.8Hz),6.25(2H,d,J=7.3Hz,1′-H)。13C-NMR数据见表1。化合物1经酸水解,TLCRf值对照，鉴定为D－木糖。以上光谱数据与　　化合物7：白色无定型粉末。ESI-MSm/z:681［M+H］+(分子式C37H60O11)。1H-NMR(Pyr)δ:0.29,0.58(each1H,d,J=3.6Hz,19-H),0.97(3H,d,J=5.9Hz,21-H),1.07,1.20,1.23,1.33,1.48,1.52(each3H,s，6×CH3),2.13(3H,s,Ac),3.50(1H,dd,J=11.5,4.0,3-H),4.17(1H,s,15-H),4.90(1H,d,J=7.4Hz,1′-H),5.78(1H,d,J=8.0Hz,24-H)。13C-NMR数据见表1。化合物7经酸水解,TLCRf值对照，鉴定为D－木糖。以上光谱数据与