萱草花化学成分与质量控制研究
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摘要
萱草花(Hemerocallis ful va)是百合科萱草属萱草的花蕾,又名黄花菜,金针菜,在亚洲地区被作为蔬菜和药物,有上千年的历史。《本草纲目》记载萱草花可治小便赤涩,身体烦热,除酒疸；可消食,利湿热,利胸膈,安五脏,令人好欢乐,无忧,轻身明目。现代药理学证明萱草花有抗氧化,降脂,抗肿瘤,抗抑郁,镇静,改善睡眠等药理活性。其中,国内外文献报道萱草花抗氧化活性研究较多,关于抗抑郁作用药效学研究仍处于起步阶段。
萱草花化学成分研究较少,具有抗抑郁活性单体未见报道。同时,萱草花未被药典收载,仅有行业标准,临床运用受到一定的限制。因此,本课题以现代化学分离分析技术和手段对萱草花醇提液进行成分研究,根据成分研究结果初步建立药材质量控制方法。
(1)萱草花化学成分研究
采用硅胶,SephadexLH-20等分离纯化方法,从萱草花中分得了12个化合物,运用NMR,MS等鉴定了其中的9个化合物,分别为：芦丁,槲皮素,槲皮素-3-0-β-D-吡喃木糖,金丝桃苷,异槲皮苷,β-谷甾醇,琥珀酸,3-糠酸,葡萄糖。其中金丝桃苷,异槲皮苷,琥珀酸,3-糠酸为首次从萱草花中分得。
分离得到的9个化合物,经文献查阅,金丝桃苷具有抗抑郁作用。故将其作为进一步研究萱草花药材质量控制方法的指标性成分。
(2)萱草花质量控制研究
在成分研究的基础上,对萱草花质量控制进行了研究：(1)以金丝桃苷为指标性成分,建立萱草花薄层鉴别方法。(2)在薄层鉴定的基础上,利用HPLC法建立了萱草花中金丝桃苷含量测定方法,并测定了8个不同产地萱草花中金丝桃苷含量。结果表明广东萱草花中金丝桃苷含量最高,陕西萱草花金丝桃苷含量最低。(3)以含量测定方法为基础,采用HPLC法初步建立萱草花指纹图谱,方法学考察结果良好。采用相似度软件确定了10批次样品中11个共有指纹峰,并鉴定了其中4个(均为黄酮类)。
综上所述,本文进行了萱草花化学成分及质量标准研究,发现具有抗抑郁作用黄酮类成分,为萱草花抗抑郁作用提供了物质基础。并建立了萱草花药材的质量标准,为萱草花药材进一步开发和利用提供依据。
Daylily (Hemerocallis fulva) of the Liliaceae is a plantlily buds, also known as daylily as a vegetable and drugs in Asia with a thousand years of history."Compendium of Materia Medica"contains daylily can cure urinea stringent body Fanre, in addition to the wine jaundice; digestion, hot and humid Lee Xiongge, five organs,It is good and joy,worry-free,light-weight names.Modern pharmacological proves daylily flower antioxidant,lipid-loweringeffects, antitumor and neural pharmacological activity.
Daylily spends less chemical composition,and antidepressant activity monomer have not been reported.The Hemerocallis is not posted pharmacopoeia,only the industry standard, that makes lots of restriction in clinical application.Therefore,this subject studies daylily alcohol extract of constituents with modern chemical separation techniques and means.According to chemical result,the quality control method was established.
(1) Chemcal Constitution Study
Techniques as TLC,normal phase silica gel column chromatog raphy,polyamide column chromatography,sephadex column chromatography etc.hace been used to determine chemical constituents of Hemerocallis fulva;The same times, structures have been identified through making use of physical and chemical properties and spectroscopic methods. A total of13compounds are isolated,9of them are identified.There arerutin, quercetin,quercetin-3-O-β-D-xylopyranosyl, hyperoside, isoquercitrin, β-sitosterol, succinic acid,3-furoicacid, glucose. Four compounds(hyperoside, isoquercitrin, succinic acid,3-furoicacid) were isolated from the plant for the first time.
Separation of the nine compounds, through literature review, hyperin has antidepressant effects.Therefore, as further study of daylily quality control method of the index component.
(2) Daylily control Study
on the basis of the chemical study, the daylily quality control were studied:(1) To hyperin for the index components, establishment of daylily TLC method.(2) In TLC id-entification based on, using HPLC method established hypericin content determination in dalily, and determination of8different clubs in the origin of hyperin content.The results show that Guangdong Hyperoside content is the highest, Shaanxi hypericin content was the lowest, and there are the great difference of the contentsduring different origins.(3) to the content determination method for the foundation, using the method of HPLC established day lily fingerprint, method of inspection results.Using similarity software identifies a batch of10samples of11common fingerprint peaks, and3of them were identified (both Flavornoids).
In summary, this paper conducted a day lily chemical composition and quality standard research, discovery has antidepressant effects of flavonoids, Hemerocallis flower for antidepressant effects provided corporeal basis.And the establishment of day lily herbal quality standard, for further development and utilization of ramie flower herbs provide a basis.
萱草花化学成分研究较少,具有抗抑郁活性单体未见报道。同时,萱草花未被药典收载,仅有行业标准,临床运用受到一定的限制。因此,本课题以现代化学分离分析技术和手段对萱草花醇提液进行成分研究,根据成分研究结果初步建立药材质量控制方法。
(1)萱草花化学成分研究
采用硅胶,SephadexLH-20等分离纯化方法,从萱草花中分得了12个化合物,运用NMR,MS等鉴定了其中的9个化合物,分别为：芦丁,槲皮素,槲皮素-3-0-β-D-吡喃木糖,金丝桃苷,异槲皮苷,β-谷甾醇,琥珀酸,3-糠酸,葡萄糖。其中金丝桃苷,异槲皮苷,琥珀酸,3-糠酸为首次从萱草花中分得。
分离得到的9个化合物,经文献查阅,金丝桃苷具有抗抑郁作用。故将其作为进一步研究萱草花药材质量控制方法的指标性成分。
(2)萱草花质量控制研究
在成分研究的基础上,对萱草花质量控制进行了研究：(1)以金丝桃苷为指标性成分,建立萱草花薄层鉴别方法。(2)在薄层鉴定的基础上,利用HPLC法建立了萱草花中金丝桃苷含量测定方法,并测定了8个不同产地萱草花中金丝桃苷含量。结果表明广东萱草花中金丝桃苷含量最高,陕西萱草花金丝桃苷含量最低。(3)以含量测定方法为基础,采用HPLC法初步建立萱草花指纹图谱,方法学考察结果良好。采用相似度软件确定了10批次样品中11个共有指纹峰,并鉴定了其中4个(均为黄酮类)。
综上所述,本文进行了萱草花化学成分及质量标准研究,发现具有抗抑郁作用黄酮类成分,为萱草花抗抑郁作用提供了物质基础。并建立了萱草花药材的质量标准,为萱草花药材进一步开发和利用提供依据。
Daylily (Hemerocallis fulva) of the Liliaceae is a plantlily buds, also known as daylily as a vegetable and drugs in Asia with a thousand years of history."Compendium of Materia Medica"contains daylily can cure urinea stringent body Fanre, in addition to the wine jaundice; digestion, hot and humid Lee Xiongge, five organs,It is good and joy,worry-free,light-weight names.Modern pharmacological proves daylily flower antioxidant,lipid-loweringeffects, antitumor and neural pharmacological activity.
Daylily spends less chemical composition,and antidepressant activity monomer have not been reported.The Hemerocallis is not posted pharmacopoeia,only the industry standard, that makes lots of restriction in clinical application.Therefore,this subject studies daylily alcohol extract of constituents with modern chemical separation techniques and means.According to chemical result,the quality control method was established.
(1) Chemcal Constitution Study
Techniques as TLC,normal phase silica gel column chromatog raphy,polyamide column chromatography,sephadex column chromatography etc.hace been used to determine chemical constituents of Hemerocallis fulva;The same times, structures have been identified through making use of physical and chemical properties and spectroscopic methods. A total of13compounds are isolated,9of them are identified.There arerutin, quercetin,quercetin-3-O-β-D-xylopyranosyl, hyperoside, isoquercitrin, β-sitosterol, succinic acid,3-furoicacid, glucose. Four compounds(hyperoside, isoquercitrin, succinic acid,3-furoicacid) were isolated from the plant for the first time.
Separation of the nine compounds, through literature review, hyperin has antidepressant effects.Therefore, as further study of daylily quality control method of the index component.
(2) Daylily control Study
on the basis of the chemical study, the daylily quality control were studied:(1) To hyperin for the index components, establishment of daylily TLC method.(2) In TLC id-entification based on, using HPLC method established hypericin content determination in dalily, and determination of8different clubs in the origin of hyperin content.The results show that Guangdong Hyperoside content is the highest, Shaanxi hypericin content was the lowest, and there are the great difference of the contentsduring different origins.(3) to the content determination method for the foundation, using the method of HPLC established day lily fingerprint, method of inspection results.Using similarity software identifies a batch of10samples of11common fingerprint peaks, and3of them were identified (both Flavornoids).
In summary, this paper conducted a day lily chemical composition and quality standard research, discovery has antidepressant effects of flavonoids, Hemerocallis flower for antidepressant effects provided corporeal basis.And the establishment of day lily herbal quality standard, for further development and utilization of ramie flower herbs provide a basis.
引文
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[4]Yun-Lian Lin, Chung-Kuang Lu, Yeh-Jeng Huang, et al.Antioxidative Caffeoylquinic Acid and Flavonoids from Hemerocallis fulva Flowers[J].Journal of Agricultural and Food Chemistry,2011,59:8789-8795.
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[1]徐冬艳,刘斌,姜艳艳。HPLC法测定降脂宁调脂抗氧化有效部位中金丝桃苷和异槲皮苷含量[J].药物分析杂志,2011,31(7)：1260-1263.
[2]傅茂润,茅林春.黄花菜的保健功效及化学成分研究进展[J].食品与发酵工业,20062,3(10)：108-109.
[3]Robert H, Muraleedharan G.Isolation and characterization of stelladerol, a new antioxidant naphthalene glycoside, and other antioxidant glycosides from edible daylily (Hemerocallis)flowers[J] Journal of Agricultural and Food Chemistry,2002,50(1): 87-91.
[4]Yun-Lian Lin, Chung-Kuang Lu, Yeh-Jeng Huang, et al.Antioxidative Caffeoylquinic Acid and Flavonoids from Hemerocallis fulva Flowers[J].Journal of Agricultural and Food Chemistry,2011,59:8789-8795.
[5]Atega Abdel-monem M, Determination of Saponin content in certain Egyptian plants by the blood-agar hemolytic zone method Zagazig J.Pharm.Sci,1992,1 (1-2):60-67, CA:120:1280391z.
[6]Zhang Yanjun, Cichewicz, Robert H, Nair Muraleedharan G.Lipid peroxidation inhibitory compounds from daylily(Hemerocallis fulva) leaves[J].Life Science,2004, 75(6):753-763.
[7]杨中铎,李援朝.萱草根化学成分的分离与结构鉴定[J].中国药物化学杂志,2003,13(1)：34-37.
[8]王鹏,吴玉,丁靖垲.黄花菜的挥发性成分[J].云南植物研究,1994,16(4)：431-434.
[9]Lin P, Cai J B, Li J.Constituent of the essential oil of Hemerocallis flava daylily[J].Flavour and Fragarance Journal,2003,18 (6):539-541.
[10]Yang Z D,Chenel H,Li Y C.A new glycoside and a noveltype diterpene from Hemerollis fulva(L.)L.Helvetica Chimica Acta,2003,86(10):3305-3309.
[11]Tai C Y,Chen B H.Analysis and stability of carotenoids in the flowers of daylily(Hemerocallis disticha)
[12]何红平,刘复初.秋水仙碱的研究进展[J].中草药,1998,29(10)：712.
[13]Konishi T, Fujiwara Y, Konoshima T, et al.Steroidal saponins from Hemerocallis fulva var.kwanso[J].Chemical & Pharmaceutical Bulletin,2001,49(3):318-320.
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