金钗石斛化学成分的研究

1、金钗石斛化学成分的研究 李玉鹏，蒋金和，刘莹，陈业高【摘要】目的研究金钗石斛的化学成分，为说明其活性成分提供根据。方法利用乙醇进展提取，硅胶柱层析、制备薄层层析和SephadexLH-20柱层析进展别离纯化，波谱分析(核磁共振氢谱、碳谱和质谱)确定构造。结果别离并鉴定了4个化合物，分别为:satin(),gigantl(II),batatasinIII(III),stigasterl(IV)。结论化合物为首次从该植物中得到。【关键词】金钗石斛；化学成分；satinhinaAbstrat：bjetiveTstudytheheialnstituentsfrDendrbiunbileLindland

2、tbtainareunderstandingfitsativepriniples.ethdspundsereextratedithethanlandislatedbylunhratgraphynsiliagel,PTLandSephadexLH-20,andthestruturesereidentifiedbyspetrspianalysis(1HNR,13NRandEiS).ResultsFurpundserebtainedandidentifiedassatin(1),gigantl(II),batatasinIII(III)andstigasterl(IV).nlusinsatin(1)

3、asbtainedfrthisplantfrthefirsttie.1仪器与材料ZF-II型紫外分析仪上海顾村中实仪器厂、Varianat-711质谱仪、BrukerDRX-500核磁共振仪。层析硅胶青岛海洋化工厂出品，SephadexLH-20:20-80(PharaiaFineheial.,Ltd.)，高效薄层层析硅胶G板烟台化工研究院。显色剂为15%硫酸乙醇溶液，所用溶剂为工业纯，使用前重蒸。其它试剂为化学纯或分析纯，金钗石斛全草采自云南思茅，由云南英茂生物技术实验室张时刚先生鉴定。2方法金钗石斛枯燥全草(0.15kg),用工业乙醇室温浸提5次，浸出液减压浓缩得乙醇提取物(6g)。提取物

4、以石油醚醋酸乙酯(10,101,51,11,01)洗脱。薄层层析检测，合并为4个部分。Fr.2(2g)经硅胶柱层析,以石油醚醋酸乙酯(201,101,51,01)洗脱、SephadexLH-20柱层析(甲醇水溶液9:1)和制备薄层层析，得化合物III(6g)，IV(25g);Fr3(2.5g)经硅胶柱层析，以氯仿丙酮(501,201,101,51,01)洗脱，SephadexLH-20柱层析(甲醇水溶液91)，得化合物I(18g),II(12g)。3结果3.1化合物I白色晶体。EIS/z(%):240(+,100),225(49),197(45),139(18);1HNR(D3)2,500Hz

5、:9.54(1H,s,5-H),9.08(1H,s,2-H),7.66(1H,d,J=8.8,H-9),7.53(1H,d,J=8.8,H-10),7.46(1H,dd,J=7.6,7.6,H-7),7.42(1H,dd,J=7.6,2.0,H-6),7.13(1H,dd,J=7.6,2.0,H-8),7.09(1H,d,J=2.4,H-1),7.01(1H,d,J=2.4,H-3),4.17(3H,s,4-e);13NR(D3)2,125Hz:157.8(s,-4),156.8(s,-2),155.7(s,-5),137.5(s,-10a),135.4(s,-8a),130.2(d,-7),

6、127.8(d,-9),127.4(d,-10),121.5(d,-8),120.2(s,-4b),117.4(d,-6),114.0(s,-4a),108.3(d,-1),103.1(d,-3),59.1(q,4-e)。与文献对照,确定化合物的构造为satin9。3.2化合物II浅黄色油状物。EIS/z(%):274(+,54),137(100),122(22),107(9),94(16),77(11);1HNRDl3,500Hz:6.87(1H,d,J=8.0,H-5),6.72(1H,d,J=8.0,H-6),6.65(1H,s,H-2),6.34(1H,s,H-4),6.30(2H,s

7、,H-2,6),3.87(3H,s,3-H3),3.78(3H,s,5-H3),2.82(4H,1,2-H2);13NRDl3,125Hz:162.1(s,-5),157.9(s,-3),147.6(s,-3),145.8(s,-1),145.0(s,-4),135.0(s,-1),122.3(d,-6),115.5(d,-2),112.5(d,-5),109.4(d,-2),108.1(d,-6),100.4(d,-4),57.2(q,5-H3),56.6(q,3-H3),39.6(t,-2),38.5(t,-1)。与文献对照,确定化合物的构造为gigantl10。转贴于论文联盟.ll.3.

8、3化合物III浅黄色油状物，EiS/z(%):244(+,30),137(100),107(43),77(8);1HNR(D3)2,500Hz:7.12(1H,dd,J=7.7,7.7,H-3),6.73(1H,d,J=7.7,H-2),6.67(1H,d,J=7.4,H-4),6.33(1H,s,H-6),6.35(1H,s,H-4),6.26(2H,s,H-2,6),3.73(3H,s,5-H3),2.82(4H,1,2-H2);13NR(D3D3,125Hz):162.0(s,-5),159.4(s,-3),158.3(s,-5),145.1(s,-1),144.3(s,-1),130.

9、0(d,-3),120.4(d,-2),116.2(s,-6),113.7(s,-4),108.9(s,-2),106.3(s,-6),99.8(s,-4),55.3(q,5-H3),38.6(t,-1),38.2(t,-2)。与文献对照,确定化合物的构造为batatasinIII10。3.4化合物IV白色针状晶体。p138140(EtA).EIS/z(relint.)412+,(100),369(16),351(55),300(45),271(70),255(93),213(30),145(31),91(44);1HNR(Dl3,500z):0.70(3H,s,H-18),0.79(3H,d

10、,J=6.5,H-27),0.80(3H,t,J=7.5,H-29),0.84(3H,d,J=6.5,H-26),1.01(3H,s,H-19),1.02(3H,d,J=6.5,H-21),3.50(1H,H-3),5.02(1H,dd,J=15,8.5,H-23),5.15(1H,dd,J=15,8.5,H-22),5.35(1H,brd,H-6).13NR(Dl3,125z):12.0(q,-18),12.2(q,-29),19.0(q,-27),19.4(q,-19),21.1(t,-26),21.1(q,-21),21.2(t,-11),24.4(t,-15),25.4(q,-28),28.9(t,-16),29.7(d,-25),31.7(t,-2),31.9(t,-7),31.9(d,-8),36.5(s,-10),37.3(t,-1),39.7(t,-12),40.5(d,-20),42.2(d,-13),42.3(t,-4),50.2(d,-9),51.2(d,-24),56.0