绿升麻中菠萝蜜烷型三萜类成分研究.docVIP

　　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asiaticoside A (1)；asiaticoside B (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)； Cimiracemoside M (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)；Cimiracemoside H（13）；Neocimicigenosides B(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：ObjectiveTo isolate and elucidate the constituents of Actaea asiatiea. MethodsChemical constituents n chromatography (Toyopearl H,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, Cimiracemoside H, Neocimicigenosides B, 2′-O-acetyl-25-anhydrocimigenol-3-O-β-D-xylopyranoside. Conclusionpound 3～15 Actaea asiatiea. 　　Key ent（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-Pack ODS-A SH-343-5 20X250mm（YMC），Econosphere silica 10μm 22 X250mm (Alltech); 液质联用色谱仪：Alliance 2695, Quattro Micro TM ESI (S m/z: 667 ［M+Na］+ (分子式 C37H56O9)。1H-NMR ( 300 MHz, Pyr ) δ: 0.21, 0.62(each 1H, d, J= 4.0 Hz, 19-H), 0.91, 1.04, 1.14， 1.17， 1.19， 1.24, 1.30 (each 3H , 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, TLC Rf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-MS m/z: 681 ［M+H］