露水草的化学成分露水草的化学成分

目的研究露水草的化学成分。 方法应用多种色谱技术进行分离，并结合NMR,MS等波谱解析确定其化学结构。结果分离得到6个化合物，鉴定为20，22-异丙叉基筋骨草甾酮C（1），20，22-异丙叉基β-蜕皮甾酮（2），22-羰基筋骨草甾酮C（3），22-羰基-β-蜕皮甾酮（4），β-谷甾醇（5），胡罗卜苷（6）。结论3为一新化合物，4为一新天然产物。     

露水草中的植物甾酮类成分

为研究露水草 (CyanotisarachnoideaC .B .Clarke)中的化学成分 ,将露水草的乙醇提取液经中性Al2 O3 柱色谱 ,制备性薄层色谱 ,高效液相色谱分离得到 3种植物甾酮类成分 ,根据理化常数和波谱数据分析进行结构鉴定 ,3个化合物分别为罗汉松甾酮C(podecdysoneC) (1) ,土克甾酮(Turkesterone) (2 ) ,β 蜕皮甾酮 (β ecdysone) (3)。其中化合物 1、2为从该植物中首次分离得到。     

牛膝的化学成分

目的研究中药牛膝的化学成分。方法采用大孔树脂、硅胶柱色谱、制备型HPLC色谱等方法分离中药牛膝中的化学成分,依据这些化合物的理化性质和1H-NMR1、3C-NMR等波谱数据进行结构鉴定。结果从牛膝中分离鉴定了5个化合物,分别为:旌节花甾酮A(stachysterone A,1)、podecdysone C(2)、β-蜕皮甾酮(β-ecdysterone,3)、25-R-膝甾酮(25-R-inokosterone,4)、25-S-牛膝甾酮(25-S-inokosterone,5)。结论化合物1、2为首次从牛膝中分离得到。     

祁州漏芦中的植物甾酮类成分

自祁州漏芦 (Rhaponticumuniflorum (L .)DC .)的根中分离得到 4种植物甾酮类成分 ,根据理化常数和波谱数据鉴定为蜕皮甾酮 (ecdysterone) (1) ,筋骨草甾酮C(ajugasteroneC) (2 ) ,蜕皮甾酮 3 O β D 葡萄糖苷 (ecdysterone 3 O β D glucopyranoside) (3) ,蜕皮甾酮 2 5 O β D 葡萄糖苷(ecdysterone 2 5 O β D glucopyranoside) (4) ,其中化合物 3,4,为从本属植物中首次分离     

双外标校准高效液相色谱法同时测定中药牛膝中皂苷类成分和甾酮类成分

牛膝现行的质量标准难以有效控制其质量。本研究运用双外标结合校正因子,同时测定牛膝中牛膝皂苷C、牛膝皂苷D、β-蜕皮甾酮、25R-牛膝甾酮和25S-牛膝甾酮的含量。采用Agilent Poroshell 120 EC-C18 (150 mm×4.6 mm, 2.7μm)色谱柱,流动相为0.1%磷酸乙腈-0.1%磷酸水溶液梯度洗脱,流速0.8 mL·min-1,柱温35℃,进样量5μL,分析时间30 min。分别以β-蜕皮甾酮和牛膝皂苷D为对照,计算25R-牛膝甾酮、25S-牛膝甾酮和牛膝皂苷C的相对校正因子(relative correction factors, RCF)和相对保留时间(relative retention time, RRT), 25R-牛膝甾酮、25S-牛膝甾酮和牛膝皂苷C的相对校正因子分别为1.116、1.056和0.888 1,不同条件下RCF稳定性良好。分别使用外标法和双外标校准法对20批不同来源牛膝样品的含量进行计算,两种方法所得结果相对误差(relative error, RE)小于5%,表明建立的双外标校准法同时测定牛膝中5种成分准确可行。含量测定结果显...     

黏萼蝇子草蜕皮甾酮类成分的分离与鉴定

目的对黏萼蝇子草根的化学成分进行研究。方法采用反复硅胶柱色谱、Sephadex LH-20柱色谱和反相半微量制备型高效液相色谱分离纯化,根据ESI-MS、1H-NMR和13C-NMR等谱学数据进行结构鉴定。结果从黏萼蝇子草根的乙醇提取物分离得到5个蜕皮甾酮类化合物,分别鉴定为20-羟基蜕皮激素(20-hydroxyecdysone,1)、1-epi-integristerone A(2)、abutasterone(3)、旌节花甾酮A(stachysterone A,4)和15-羟基旌节花甾酮A(15-hydroxystachysterone A,5);另外得到胡萝卜苷(daucosterol,6)和β-谷甾醇(β-sitosterol,7)2个甾醇类化合物。结论化合物2-5为蝇子草属植物中首次分离的化合物。     

小百部的甾体皂甙成分

从云南产小百部(Asparagus filicinus Buch.-Ham)的根中分离到四个甾体皂甙,经光谱分析和化学降解,确定了结构,其中三个为新化合物,分别命名为小百部甙A(Ⅰ),小百部甙B(Ⅱ)和小百部甙C(Ⅲ)。另一个为已知皂甙Asp-Ⅳ的22-甲氧基化物(Ⅳ)。此外还分离到β-蜕皮甾酮(β-ecdysone,Ⅴ)。     

祁州漏芦蜕皮甾酮类化学成分的研究

从祁州漏芦[Rhaponticum uniflorum(L.)DC.]的根中,分离出三个蜕皮甾酮类化合物Ⅰ,Ⅱ,Ⅲ,其中Ⅱ根据UV,IR,MS,¹³CNMR,¹HNMR,¹H-¹HCOSY,¹H-¹HNOESY,¹H-¹³C COSY,及CD谱确定其结构为(20R,22R,24S)-2β,3β,11α,14α,20,22,24-heptahydroxy-5β-cholest-7-en-6-one,为一新化合物,命名为漏芦甾酮(rhaponfisterone)。化合物Ⅰ和Ⅲ分别鉴定为蜕皮甾酮(ecdysterone)和土克甾酮(turkesterone)。     

在体单向灌流法研究β-蜕皮甾酮大鼠在体肠吸收特性

目的考察β-蜕皮甾酮的肠道吸收特性,探究β-蜕皮甾酮生物利用度低的原因。方法采用大鼠在体单向肠灌流模型,运用HPLC法测定药物浓度。分别考察小肠吸收部位(十二指肠、空肠、回肠、结肠),药物浓度,灌流液pH值,肠道菌群对β-蜕皮甾酮吸收的影响。结果β-蜕皮甾酮在不同肠段的吸收速率常数(K_a)由高到低依次为回肠、结肠、空肠、十二指肠;以β-蜕皮甾酮浓度为50、100、200μg·mL~(-1)的含药缓冲液在空肠进行吸收实验,K_a和小肠有效渗透系数(P_(eff))差异无统计学意义;药物的吸收程度在空肠随pH值升高而增加;大鼠肠道菌群失衡会干扰β-蜕皮甾酮的吸收。结论β-蜕皮甾酮在各个肠段均有吸收,但在肠道下部吸收较好;吸收机制为被动扩散;药物在碱性环境下吸收较好;肠道菌群对β-蜕皮甾酮吸收有显著影响。     

β-蜕皮甾酮化学结构修饰研究进展

β-蜕皮甾酮是一种重要的植物甾酮,它参与控制昆虫等无脊椎动物的蜕皮和繁殖过程。药理实验表明β-蜕皮甾酮具有促进蛋白质合成、降低血糖血脂以及改善学习和记忆等多种功效。多年来人们对其化学结构修饰及蜕皮活性的研究取得了一定的进展和成果,该文对历年来β-蜕皮甾酮的化学结构修饰和蜕皮活性研究成果进行概述。     

Ecdysteroids from Rhaponticum uniflorum.

Five phytoecdysteroids were isolated from the roots of Rhaponticum uniflorum. They were identified as ecdysterone, ajugasterone C, ajugasterone C-20,22-monoacetonide, ajugasterone C-2,3,20,22-diacetonide and 5-deoxykaladasterone-20,22-monoacetonide by means of spectroscopic data. This is the first report of ajugasterone C-2,3,20,22-diacetonide and 5-deoxykaladasterone-20,22-monoacetonide isolated from a natural source.     

Phytoecdysteroids of Diploclisia glaucescens Seed

Five phytoecdysteroids were isolated from the seeds of DIPLOCLISIA GLAUCESCENS and identified by spectrometric methods ( (1)H-NMR, (13)C-NMR and CIMS). One of them, 24- EPI- makisterone A, has not been reported before. The other four - 20-hydroxyecdysone, makisterone A, 24(28)-dehydromakisterone A and pterosterone - were known previously. The (13)C-NMR spectrum of 24(28)-dehydromakisterone A is presented for the first time.     

Simultaneous determination of eight components in Radix Tinosporae by high-performance liquid chromatography coupled with diode array detector and electrospray tandem mass spectrometry

High-performance liquid chromatography (HPLC) coupled with electrospray tandem mass spectrometry (ESI-MS-MS) and diode array detection (DAD) was used to identify and simultaneously determine eight major ingredients in Radix Tinosporae. The assay was performed on a Diamonsil C(18) analytical column with a gradient solvent system of A (water containing 0.2% formic acid, 20mM ammonium acetate) and B (methanol/acetonitrile=1/1, v/v). The 217, 248, 270 and 347 nm, respectively, were chosen as the monitoring wavelengths to determine four structural types of components, say columbin, phytoecdysteroids (including 20-hydroxyecdysone, 2-deoxy-20-hydroxyecdysone 3-O-beta-d-glucopyranoside and 2-deoxy-20-hydroxyecdysone), menisperine and protoberberine alkaloids (including columbamine, jatrorrhizine and palmatine). This method was validated in respect to precision, repeatability and accuracy, and was successfully applied to quantify the eight components in 39 batches of R. Tinosporae for quality control purpose. The results indicated that the proposed method could be readily utilized as a quality control method for traditional Chinese medicine (TCM).     

New Ecdysteroids from Serratula tinctoria

Six new ecdysteroids have been isolated from SERRATULA TINCTORIA; these are: the 2,22- and 3,22-diacetates of 20-hydroxyecdysone, 5beta-hydroxyrubrosterone, 3-epi-poststerone, 3-epi-rubrosterone, and 22-oxo-20-hydroxyecdysone. These minor compounds were found together with the known ecdysteroids, 20-hydroxyecdysone, its 2-, 3-, and 22-monoacetates, rubrosterone, poststerone, polypodine B (5beta,20-dihydroxyecdysone), pterosterone (25-deoxy-20,24-dihydroxyecdysone), and makisterone C (24-ethyl-20-hydroxyecdysone). All these ecdysteroids were isolated by a combination of several chromatographic techniques (liquid chromatography on alumina, DCCC, and HPLC), then identified using standard mass spectrometric and 2D (1)H-NMR techniques.     

Analysis of phytoecdysteroids in cultured plants of Ajuga nipponensis makino

Cultured plants of Ajuga nipponensis contained cyasterone (1), ajugasterone C (2), cyasterone-22-acetate (3) and 22-dehydrocyasterone (4) based on HPLC and NMR data, whereas 20-hydroxyecdysone was not detectable. The presence of compounds 2-4 is reported for the first time in this species. Compound 1 is the main phytoecdysteroid component found in both preblossom and blossom plants, but the latter contained higher amount than the former. Compared with other parts of the plant, the highest percentage of 1 and 3 occurred in leaves, amounting to 60.1% and 88.0% respectively, whereas the flowers contained mainly 2, which represented 72.8% of the total amount in whole plant. The contents of phytoecdysteroids in stems were very low.     

Analysis of Phytoecdysteroids in Cultured Plants of Ajuga Nipponensis Makino

Abstract

Cultured plants of Ajuga nipponensis contained cyasterone (1), ajugasterone C (2), cyasterone-22-acetate (3) and 22-dehydrocyasterone (4) based on HPLC and NMR data, whereas 20-hydroxyecdysone was not detectable. The presence of compounds 2–4 is reported for the first time in this species. Compound 1 is the main phytoecdysteroid component found in both preblossom and blossom plants, but the latter contained higher amount than the former. Compared with other parts of the plant, the highest percentage of 1 and 3 occurred in leaves, amounting to 60.1% and 88.0% respectively, whereas the flowers contained mainly 2, which represented 72.8% of the total amount in whole plant. The contents of phytoecdysteroids in stems were very low.     

Structural diversity of ecdysteroids of Lychnis flos-cuculi

Eleven ecdysteroids have been isolated from Lychnis floscuculi; we are the first who report eight ecdysteroids of the eleven compounds in this plant. Two of these ecdysteroids, dihydrorubrosterone and 20-hydroxyecdysone 3-acetate are newly discovered natural products. The success of isolation of these new ecdysteroids has been based on the use of separation methods in a proper order; these separation procedures were completing each others. At the beginning steps of isolation simple separation methods were used, such a solvent-solvent distribution and fractionated precipitation. Two third of the contaminants were removed thereby. High capacity low resolution methods were used then, such as classical adsorption column chromatography and preparative thin-layer chromatography. The major component (20-hydroxyecdyssone) and certain minor ecdysteroids (polypodine B and rubrosterone) were isolated in pure form here. Purification of the further minor components (poststerone, 2-deoxy-20-hydroxyecdysone, vitikosterone E, dihydrorubrosterone, makisterone A, taxisterone, 20-hydroxyecdysone 2-acetate, 20-hydroxyecdysone 3-acetate) required HPLC and other absorption chromatographic methods. Our recent separation scheme means a generally applicable guiding principle for isolation of any plant ecdysteroid, major and minor alike. Structural identification of the known ecdysteroids was based on their spectral data and that of their literature information. Structural elucidation of 20-hydroxyecdysone 3-acetate was done by the help of a standard component prepared by acetylation of 20-hydroxyecdysone. From the mixture of seven acetates the corresponding compound (20-hydroxyecdysone 3-acetate) was isolated, and used for identification. Structural diversity of ecdysteroids of Lychnis flos-cuculi is evaluated, and a tentative explanation is introduced for the formation and biosynthesis of the versatility of phytoecdysteroids.     

Phytoecdysteroid constituents from Cyanotis arachnoidea

Four phytoecdysteroids that have only 19 or 21 carbons, named 11alpha-hydroxyrubrosterone (1), dihydroxyrubrosterone (2), rubrosterone (3) and poststerone (4), were isolated from the whole plant of Cyanotis arachnoidea C.B. Clarke. Among them, 1 was a new compound. Their structures were elucidated by spectroscopic methods.