商陆皂苷的化学成分及2010版《中国药典》商陆质量标准的修订研究
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摘要
商陆是一种传统中药,为商陆科商陆属植物商陆(Phytolacca esculenta Van Houtte或P.acinosa Roxb.)和美洲商陆(P.americana L.)的根的炮制品,被历版中国药典收录。商陆始载于《本经》,被列为下品,其味苦,性寒,有毒,归肺、脾、肾、大肠经。功能逐水消肿,通利二便；外用解毒散结。用于水肿胀满,二便不通；外治痈肿疮毒。
商陆的主要成分有商陆多糖、蛋白质和三萜皂苷等,其中商陆皂苷具有抗炎、抗肿瘤、调节免疫等多种药理活性,商陆皂苷甲更是有望成为一种潜在的治疗机体自身免疫疾病的药物。为了更方便地获得商陆皂苷以开展后期工作,本文研究并优化了了商陆皂苷的分离方法。
本论文包括以下工作：
首先对近30年国内外有关商陆的研究成果进行概括,包括植物学特征、炮制、化学成分及其分离纯化方法、含量测定、药理作用、临床应用和毒性等。
第二,进行了商陆皂苷的分离和纯化研究：1.通过多种色谱手段,从商陆根中分离得到7个单体化合物,分别是：胡萝卜苷、商陆皂苷乙、商陆皂苷丁、商陆皂苷T、商陆皂苷丙、商陆皂苷甲、商陆皂苷H,其中商陆皂苷T为新发现的化合物。2.探索了商陆中商陆皂苷甲对照品的分离制备工艺,以期能够大批量获得高纯度的商陆皂苷甲对照品,并起草了商陆皂苷甲对照品的质量标准以期保证其质量水平。3.将HSCCC与ELSD联用从商陆乙酸乙酯粗提物中分离出高纯度的商陆皂苷甲、商陆皂苷乙、商陆皂苷丙和商陆皂苷丁,为实现商陆皂苷的快速高效分离提供了较为理想的参考。
本专题还包括《中华人民共和国药典》2010版(Ⅰ部)标准研究课题：商陆的质量标准修订。实验采用专属性的HPLC-ELSD法来测定不同产地商陆药材、商陆饮片及醋商陆中商陆皂苷甲的含量,并制定了商陆皂苷甲的含量限度；描述了商陆饮片和醋商陆的性状,制定了薄层鉴别方法,测定了多批醋商陆浸出物、水分、酸不溶性灰分的含量并确立了相关限度。根据以上工作结果,作者修订了2010版《中国药典》(Ⅰ部)商陆项的质量标准,该研究结果以经通过国家药典委员会审核,成为药典正文。
Radix Phytolaccae(Chinese name shanglu),a famous Chinese herbal medicine collected in Chinese pharmacopoeia,is derived from the root of Phytolacca acinosa Roxb.or P.americana L.. It has been long used for treatment of edema,abdominal fullness,dysuria,abnormal defecation,and external application for the treatment of carbuncles and sores as a traditional Chinese medicine(TCM).
The major constituents of R. Phytolaccae are PEPs,protein and triterpene saponins. The major biological activity of the compounds in R. Phytolaccae is attributed to its triterpene saponins, which have been reported to have a variety of activities such as induction of immune interferon(INF-c),anti-inflammatory agents,and tumor necrosis factor(TNF);enhancement of leukocyte phagocytosis and promotion of DNA transformation;antifertility;and molluscicidal,etc.For supplying a more convenient method to get these saponins,we did lots of relative researches as following aspects:
Firstly we summarized the researches on R. Phytollaccae in recent 30 years,including the plant,preparing,constituents,content determine,bio-activities and toxicity.
The second part is the separation and purification of crude saponins from the roots of R. Phytolaccae:(1)By using several chromatographic methods,we got 7 compounds:daucosterol,esculentoside B, esculentoside D, esculentoside C, esculentoside T, esculentoside A(EsA) and esculentoside H, esculentoside T is a new compound. (2)In order to get large number of EsA quickly,the procedure of separation and purification of EsA was also investigated.As a CRS in pharmacopoeia, EsA was added a criterion by us. (3)We established a method for the purification of four saponins such as esculentosides A-D from a crude extract of R. Phytolaccae by HSCCC coupled with an evaporative light scattering detector.
Meanwhile we assumed one standard research Project of Pharmacopoeia of People's Republic of China Edition 2010:Quality specification revision of R. Phytolaccae.A special HPLC-ELSD method was adopted for the determination of EsA in medical material and processed product of R.Phytolaccae from different places,then a content limitation was established.We described the shape and properties of R. Phytolaccae and established a TLC method in order to distinguish the medical material.Lastly the limitations of water content,acid-insoluble ash content and extractives of R. Phytolaccae(processed with vinegar) were established.On the base of the studies above,the quality specification of R. Phytolaccae was successfully revised.
商陆的主要成分有商陆多糖、蛋白质和三萜皂苷等,其中商陆皂苷具有抗炎、抗肿瘤、调节免疫等多种药理活性,商陆皂苷甲更是有望成为一种潜在的治疗机体自身免疫疾病的药物。为了更方便地获得商陆皂苷以开展后期工作,本文研究并优化了了商陆皂苷的分离方法。
本论文包括以下工作：
首先对近30年国内外有关商陆的研究成果进行概括,包括植物学特征、炮制、化学成分及其分离纯化方法、含量测定、药理作用、临床应用和毒性等。
第二,进行了商陆皂苷的分离和纯化研究：1.通过多种色谱手段,从商陆根中分离得到7个单体化合物,分别是：胡萝卜苷、商陆皂苷乙、商陆皂苷丁、商陆皂苷T、商陆皂苷丙、商陆皂苷甲、商陆皂苷H,其中商陆皂苷T为新发现的化合物。2.探索了商陆中商陆皂苷甲对照品的分离制备工艺,以期能够大批量获得高纯度的商陆皂苷甲对照品,并起草了商陆皂苷甲对照品的质量标准以期保证其质量水平。3.将HSCCC与ELSD联用从商陆乙酸乙酯粗提物中分离出高纯度的商陆皂苷甲、商陆皂苷乙、商陆皂苷丙和商陆皂苷丁,为实现商陆皂苷的快速高效分离提供了较为理想的参考。
本专题还包括《中华人民共和国药典》2010版(Ⅰ部)标准研究课题：商陆的质量标准修订。实验采用专属性的HPLC-ELSD法来测定不同产地商陆药材、商陆饮片及醋商陆中商陆皂苷甲的含量,并制定了商陆皂苷甲的含量限度；描述了商陆饮片和醋商陆的性状,制定了薄层鉴别方法,测定了多批醋商陆浸出物、水分、酸不溶性灰分的含量并确立了相关限度。根据以上工作结果,作者修订了2010版《中国药典》(Ⅰ部)商陆项的质量标准,该研究结果以经通过国家药典委员会审核,成为药典正文。
Radix Phytolaccae(Chinese name shanglu),a famous Chinese herbal medicine collected in Chinese pharmacopoeia,is derived from the root of Phytolacca acinosa Roxb.or P.americana L.. It has been long used for treatment of edema,abdominal fullness,dysuria,abnormal defecation,and external application for the treatment of carbuncles and sores as a traditional Chinese medicine(TCM).
The major constituents of R. Phytolaccae are PEPs,protein and triterpene saponins. The major biological activity of the compounds in R. Phytolaccae is attributed to its triterpene saponins, which have been reported to have a variety of activities such as induction of immune interferon(INF-c),anti-inflammatory agents,and tumor necrosis factor(TNF);enhancement of leukocyte phagocytosis and promotion of DNA transformation;antifertility;and molluscicidal,etc.For supplying a more convenient method to get these saponins,we did lots of relative researches as following aspects:
Firstly we summarized the researches on R. Phytollaccae in recent 30 years,including the plant,preparing,constituents,content determine,bio-activities and toxicity.
The second part is the separation and purification of crude saponins from the roots of R. Phytolaccae:(1)By using several chromatographic methods,we got 7 compounds:daucosterol,esculentoside B, esculentoside D, esculentoside C, esculentoside T, esculentoside A(EsA) and esculentoside H, esculentoside T is a new compound. (2)In order to get large number of EsA quickly,the procedure of separation and purification of EsA was also investigated.As a CRS in pharmacopoeia, EsA was added a criterion by us. (3)We established a method for the purification of four saponins such as esculentosides A-D from a crude extract of R. Phytolaccae by HSCCC coupled with an evaporative light scattering detector.
Meanwhile we assumed one standard research Project of Pharmacopoeia of People's Republic of China Edition 2010:Quality specification revision of R. Phytolaccae.A special HPLC-ELSD method was adopted for the determination of EsA in medical material and processed product of R.Phytolaccae from different places,then a content limitation was established.We described the shape and properties of R. Phytolaccae and established a TLC method in order to distinguish the medical material.Lastly the limitations of water content,acid-insoluble ash content and extractives of R. Phytolaccae(processed with vinegar) were established.On the base of the studies above,the quality specification of R. Phytolaccae was successfully revised.
引文
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