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作 者:娄京荣 郑重飞[2] 李莹[2] 亓超 崔雪 姚庆强[2] LOU Jing-rong;ZHENG Zhong-fei;LI Ying;QI Chao;CUI Xue;YAO Qing-qiang(School of Medicine and Life Sciences,University of Ji'nan,Shandong Academy of Medical Sciences,Ji'nan 250200,China;Institute of Materia Medica,Shandong Academy of Medical Sciences,Key Laboratory for Biotech-Drugs Ministry of Health,Key Laboratory for Rare&Uncommon Diseases of Shandong Province,Ji'nan 250062,China)
机构地区:[1]济南大学,山东省医学科学院医学与生命科学学院,济南250200 [2]山东省医学科学院药物研究所国家卫生部生物技术药物重点实验室,山东省罕少见病重点实验室,济南250062
出 处:《中国实验方剂学杂志》2020年第10期141-147,共7页Chinese Journal of Experimental Traditional Medical Formulae
基 金:山东省重点研发计划项目(2017YYSP035)。
摘 要:目的:对95%,75%乙醇提取花椒茎的化学成分进行分离和鉴定。方法:取花椒茎25 kg,经95%乙醇,75%乙醇加热回流提取3次,过滤后浓缩成浸膏。95%乙醇提取得到的浸膏,分别用石油醚、二氯甲烷、乙酸乙酯、正丁醇萃取,各萃取部分与75%乙醇提取得到的浸膏经反复硅胶柱色谱,LH-20型羟丙基葡聚糖凝胶(Sephadex LH-20)柱色谱,C18柱色谱,中压制备,重结晶等方法分离纯化,用质谱、核磁等波谱技术进行鉴定。结果:分离得到的16个化合物分别为白鲜碱(1),德卡林碱(2),花椒棚碱(3),伪非洲防己碱(4),茵芋碱(5),去甲白屈菜红碱(6),欧芹酚(7),白蜡树素(8),3,4,5-三甲氧基肉桂醇(9),细辛脂素(10),丁香树脂二甲醚(11),丁香树脂酚(12),刚果荜澄窃脂素(13),邻苯二酸双(2-乙基己基)酯(14),24-propylcholesterol(15),蔗糖(16)。结论:化合物伪非洲防己碱(4),3,4,5-三甲氧基肉桂醇(9),24-propylcholesterol(15)为花椒属中首次分离,化合物白鲜碱(1),欧芹酚(7),白蜡树素(8),细辛脂素(10),丁香树脂二甲醚(11),丁香树脂酚(12),刚果荜澄窃脂素(13),邻苯二酸双(2-乙基己基)酯(14)为花椒中首次分离。Objective:To isolate and identify the chemical constituents from the 95%,75%ethanol extracts of the stems of Zanthoxylum bungeanum.Method:The 25 kg stems of Z.bungeanum were extracted with95%,75%ethanol for three times,and the combined filtrates were concentrated under vacuum to get the extracts.The 95%extracts were then extracted by petroleum ether,dichloromethane,ethyl acetate and n-butanol successively to obtain corresponding fractions.Such fractions and 75%extracts were isolated and purified by silicagel,Sephadex LH-20,ODS,preparation HPLC and recrystallization to obtain compounds.Their structures were identified by mass spectroscopy(MS),and nuclear magnetic resonance(NMR).Result:Sixteen compounds were isolated from the stems of Z.bungeanum and identified as dictamnine(1),decarine(2),zanthobungeanine(3),pseudocolumbamine(4),skimmianine(5),norchelerythrine(6),osthenol(7),dimethylfraxetin(8),3,4,5-trimethoxycinnamylalcohol(9),asarinin(10),yangambin(11),syringaresinol(12),ashantin(13),bis(2-ethylhexyl)benzene-1,2-dicarboxylate(14),24-propylcholesterol(15),and sucrose(16).Conclusion:Compounds pseudocolumbamine(4),3,4,5-trimethoxycinnamylalcohol(9),and 24-propylcholesterol(15)were isolated from the genus of Zanthoxylum for the first time and compounds dictamnine(1),osthenol(7),dimethylfraxetin(8),asarinin(10),yangambin(11),syringaresinol(12),ashantin(13),and bis(2-ethylhexyl)benzene-1,2-dicarboxylate(14)were isolated from this plant for the first time.
关 键 词:花椒茎 生物碱 香豆素 木脂素 醇提物 伪非洲防己碱 3 4 5-三甲氧基肉桂醇 24-propylcholesterol
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