鬼箭锦鸡儿化学成分的研究

1、H20O7相比较,基本一致10,确定该化合物为42O2 (42methoxycinnamoy22L2rhamnopyranose。化合物:白色无定形粉末,光谱数据与文献中Linarin一致,TLC3种展开剂系统展开,与linarin 标准品相比较,Rf值一致11,故确定化合物为linarin。化合物:白色无定性粉末,Libermann2Bur2 chard和Molish反应均为阳性,IR图谱与2胡萝卜苷(Daucosterin标准品一致,与2胡萝卜苷标准品混合后熔点不下降,TLC3种展开剂系统展开,与2胡萝卜苷相比较,Rf值一致,将该化合物的1HNMR 和13CNMR图谱数据与文献中报道的2胡

2、萝卜苷相比较,基本一致12。故确定化合物为2胡萝卜苷。R eferences:1Houtghon J,Candau M1Phenylpropanoid glycosides in B uddle2ja davi diiJ1N at Product,1985,48(6,1005210071 2Institutum Botanicum Kunmingense Academiae Sinicae Edita.Flora Y unnanica(云南植物志M1Tomus3,Kunming:Yunnan Science and Technology Publishing House,1977. 3Lu J

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4、,1975,31(7:24472244915Houghton P L1Phenolic fatty acid esters from B uddleja globosastembarkJ1Phytochemist ry,1989,28(10:269316Zeng G,Liu C J,Meng B H1Studies on the ethyl acetate partialfrom stembark of Prena f ulca CraibJ1Chi n Tradit HerbDrugs(中草药,1990,21(5:821117Rao G X,Lin Z W,Sun H D1Chemical

5、constituents ofPeucedanum decumbensJ1Acta Bot Y unnan(云南植物研究,1990,12(3:335233918K ong L Y,Min Z D1Studies on the chemical constituents ofstem and leaf of Com mon Poi nsettia(Euphorbia pulcherri maJ1Chi n Tradit Herb Drugs(中草药,1996,27(8:4452 44719Zhou Z Y,Y ang C R1Saluenin,a new flavonol glycoside f

6、romCamellia sal uenenisJ1Acta Bot Y unnan(云南植物研究,2000,22(1:90296110Zhang W J,Liu Y Q,Li X C1Chemical constituents from Scro2phularia ni ngpiensisJ1Acta Bot Y unnan(云南植物研究,1994,16(4:4072412111Zhang H Y,Pan J X1Phenylpropanoid glycosides and flavonoidglycosides isolated from buds of B uddleja of f ici

7、 nalis MaximJ1J Chi n Pharm Sci,1996,5(2:1052108112Tu P F,He Y,Lou Z1Studies on the chemical constituents ofthe cultivated Desertlivi ng cistanche(Cistanche deserticolaJ1N at Prod Res Dev(天然产物研究与开发,1997,9(6:72101鬼箭锦鸡儿化学成分的研究杨敬芝1,李建北1,张万隆2,丁怡1(11中国医学科学院中国协和医科大学药物研究所,北京100050;21北京卫生学校,北京100053鬼箭锦鸡儿Car

8、agana j ubata(Pall1Poir1,又名冠毛绵鸡儿,为豆科植物。分布在我国辽宁、河北、山西、内蒙古、四川和西北等地。具有接筋续断、祛风利湿、活血通络、消肿止痛。治跌打损伤、风湿筋骨疼痛、月经不调、乳房发炎1。已有文献报道了其中的几个黄酮类化合物2,为寻找活性成分,我们对其化学成分进行了系统研究,从其枝叶的乙醇提取物中,采用大孔吸附树脂、Sephadex L H220、正相及反相硅胶柱层析,分离得到5个化合物。根据光谱数据鉴定其结构,分别是白黎芦醇(,scir2 pusin B(,cassigarol E(,427二羟基232甲氧基黄酮(,4,72二羟基232甲氧基异黄酮(,化合物

9、为首次从该种植物中分离得到。1仪器与材料Boetius熔点测定仪,温度计未校正。ZAB22F 型MA T质谱仪。岛津UV2240型紫外光谱仪。AM500型和Mercury300型核磁共振仪。薄层层析硅胶(GF254,1040目和柱层层析硅胶(300 400目均为青岛海洋化工厂产品。RA型大孔吸附树脂为北京化工厂产品。C18反相硅胶为Unicorn 公司产品。鬼箭锦鸡儿C1j ubata(Pall1Poir1采自青海,由兰州大学生物系张国良教授鉴定。2提取分离鬼箭锦鸡儿全草112kg,用95%乙醇回流提取3次(2h/次,浓缩得总浸膏150g,通过RA型大孔吸附树脂柱,30%,50%,70%,95

10、%乙醇梯度洗脱,54中草药Chinese Traditional and Herbal Drugs第34卷第5期2003年5月收稿日期:2002207205基金项目:北京市科委“248”生物医药基地项目(9550214900作者简介:杨敬芝,女,主管技师,从事天然产物研究,已发表论文4篇。Tel:(01063165227洗脱液浓缩至干,分别得到各个部分。50%乙醇部分44g 通过硅胶柱(200300目,以三氯甲烷2甲醇(81洗脱,等份切割成7份,分别用乙醇洗脱,收集洗脱液浓缩至干,分别得到各个部分。第6部分通过硅胶H 柱,环己烷2乙酸乙酯2丙酮(311洗脱得到化合物。第3部分通过硅胶柱(200

11、300目,三氯甲烷2甲醇(121洗脱,其中1315份合并后通过L H 220柱得到化合物,3141份合并后通过L H 220柱得到化合物。第7部分通过500g 硅胶柱(200300目,环己烷2乙酸乙酯2丙酮(411洗脱,等分切割成7份,分别用乙醇洗脱,收集洗脱液浓缩至干,分别得到各个部分。第3份通过反相C 18柱,甲醇2水(11洗脱,得到化合物,第5份通过80g 反相C 18柱,甲醇2水(11洗脱,得到化合物。3结构鉴定化合物:无色针晶,mp 254255,EI 2MS m/z (%:228M +(100。UV max (MeOH (nm :230(sh ,335(MeOH 。与白藜芦醇对照,

12、在多种溶剂系统中TLC 的Rf 值完全一致,故推定化合物为白藜芦醇。化合物:浅黄色无定型粉末,经醋酐吡啶乙酰化,得到乙酰化产物。乙酰化物的FAB 2MS m/z (%:780M +,738,696,654,612,570。1HNMR (500MHz ,CD 3COCD 3:4144(1H ,d ,J =418Hz ,5133(1H ,d ,J =418Hz ,6121(3H ,brs ,6131(1H ,d ,J =211Hz ,6167(1H ,d ,J =1615Hz ,6170(4H ,brs ,6179(1H ,d ,J =810Hz ,6181(1H ,d ,J =210Hz ,61

13、85(1H ,brs ,6186(1H ,d ,J =1615Hz 。13CNMR (300MHz ,CD 3COCD 3:5712,9411,9619,10213,10414,107102,11315,11412,11612,11613,11813,11918,12010,12317,13017,13018,13512,13616,14610,146112,14613,14718,15917,160102,16217。以上数据与文献报道的scirpusin B 一致3,4,故确定化合物为scirpusin B 。化合物:浅黄色无定型粉末,FAB 2MS m/z(%:486(60。1HNMR

14、(500MHz ,CD 3COCD 3:4188(2H ,s ,6125(2H ,d ,J =210Hz ,6128(1H ,t ,J =210Hz ,6130(1H ,t ,J =210Hz ,6159(2H ,d ,J=210Hz ,6161(1H ,dd ,J =210,810Hz ,6174(1H ,dd ,J =310,810Hz ,6181(1H ,d ,J =210Hz ,6196(1H ,d ,J =815Hz ,6199(1H ,d ,J =1612Hz ,6130(1H ,d ,J =1612Hz ,7114(1H ,dd ,J =210,815Hz ,7120(1H ,d

15、 ,J =2Hz 13CNMR (300MHz ,CD 3COCD 3:8111,8115,10310,10316,105192,107152,11515,11518,11610,11810,12018,12019,12813,12819,12914,13212,14010,14018,14419,14513,14518,14613,159122,159172。以上数据与文献报道的cassigarol E 一致5,故确定化合物为cassigarol E 。化合物:浅黄色结晶,EIMS ,1HNMR 数据与文献报道的7,42二羟基232甲氧基黄酮(一致6,故确定化合物为7,42二羟基232甲氧基

16、黄酮(。化合物:浅黄色结晶,EIMS ,1HNMR 数据与文献报道的7,42二羟基232甲氧基异黄酮(一致2,故确定化合物为7,42二羟基232甲氧基异黄酮(。R eferences :1Jiangsu New Medical College 1Dictionary of Chi nese M ateriaMedica (中药大辞典M 1Shanghai :Shanghai Science andTechnology Publisher ,198612Wang Y L ,Chen W M ,Li G Y 1Studies on the chemical con 2stituents from

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