白树中二萜类成分的分离与鉴定

目的对白树(Suregada glomerulata(Bl.)Baill.)的化学成分进行研究,为进一步开发利用该植物资源提供依据。方法通过硅胶柱色谱、ODS柱色谱和制备HPLC等手段对白树进行分离和纯化,利用理化性质和波谱数据进行结构鉴定。结果从白树枝叶中分离得到12个二萜,分别鉴定为3α,17-dihydroxy-ent-pimara-8(14),15-diene(1)、3β-acetoxy-1-one-8β,14α-epoxy-13,15-abiatene-16,12-olide(2)、gelomulide D(3)、gelomulide E(4)、泽漆内酯丙(helioscopinolide C,5)、3β-acetoxy-8β,14α-dihydroxy-1-one-13,15-abiatene-16,12-olide(6)、3β,6β-diacetoxy-1-one-8β,14α-epoxy-13,15-abiatene-16,12-olide(7)、gelomulide A(8)、gelomulide G(9)、泽漆内酯甲(helioscopinolide A,10)、泽漆内酯丁(helioscopinolide D,11)、泽漆内酯乙(helioscopinolide B,12)。结论化合物1为首次从白树属植物中分离得到,化合物2⁸为首次从白树中分离得到。     

温郁金中倍半萜类成分的分离与鉴定

目的对温郁金(Curcuma wenyujin)的化学成分进行研究。方法采用硅胶柱色谱、ODS柱色谱、Sephadex LH-20柱色谱,HPLC以及制备薄层色谱(P-TLC)进行分离和纯化,并依据理化性质和光谱学分析鉴定其化学结构。结果从温郁金的体积分数为50%的乙醇溶液提取物中分离得到6个倍半萜,分别鉴定为原莪术醇(procurcumenol,1)、环氧泽泻烯(alismoxide,2)、aeruginolac-tone(3)、(1E,4Z)-8-hydroxy-6-oxogermacra-1(10),4,7(11)-trieno-12,8-lactone(4)、1β,4α-di-hydroxy-5α,8β(H)-eudesm-7(11Z)-en-12,8-olide(5)和curcolonol(6)。结论其中化合物1、2为愈创木烷型倍半萜,3、4为吉玛烷型倍半萜,5、6为桉烷型倍半萜。化合物4、5均为首次从该属植物中分离得到,化合物1、2、3、6均为首次从本植物中分离得到。     

海洋真菌Aspergillus sp. SCS-KFD03化学成分研究

目的 对海洋真菌Aspergillus sp. SCS-KFD03的发酵液中化学成分进行分离鉴定,并测定其生物活性。 方法 采用硅胶柱色谱、Sephadex LH-20凝胶柱色谱和高效液相色谱等技术进行分离纯化,运用各种波谱方法对分离所得化合物进行结构鉴定,并测定化合物乙酰胆碱酯酶和α-糖苷酶抑制活性。结果 分离鉴定了9个化合物,经鉴定为phomaligol A1（1）、5-（乙酰氧基甲基）呋喃-3-酸（2）、 phomapyrone C（3）、4-羟基异苯并呋喃-1(3H)-酮（4）、penicillivinacine（5）、22(E)-5α,8α-epidioxyergosta-6,22-dien-3β-ol（6）、lucidal（7）、dankasterone A（8）、bis-(2-methylheptyl)-phthalate（9）,其中化合物4为新天然产物。化合物5、6、7和9具有较弱的乙酰胆碱酯酶抑制的活性,化合物5具有强于阳性药阿卡波糖的α-糖苷酶抑制活性,8和9的α-糖苷酶抑制活性与阳性药相当。结论 化合物1~9均为首次从海洋曲霉属真菌Aspergillus sp. SCS-KFD03中分离得到,部分化合物具有乙酰胆碱酯酶和α-糖苷酶的抑制活性。     

内生真菌Sporormiella irregularis(No.71-11-4-1)中一个新的二裂甾体

目的研究一株地衣内生真菌Sporormiella irregularis(No.71-11-4-1)的次生代谢产物。方法采用硅胶柱色谱、Sephadex LH-20凝胶柱色谱、ODS柱色谱以及HPLC等多种色谱手段对其发酵提取物进行分离纯化,并借助光谱学数据对单体化合物进行结构鉴定。结果分离得到9个甾类化合物,分别鉴定为22E-3,7-epoxy-5,10∶8,9-disecoergosta-9(10),22-diene-5,8-dione(1)、22E-5α,6α-ep-oxyergosta-8(14),22-diene-3β,7α-diol(2)、22E-5α,6α-epoxyergosta-8(9),22-diene-3β,7α-diol(3)、22E-7α-methoxy-5α,6α-epoxyergosta-8(14),22-dien-3β-ol(4)、22E-3β-hydroxy-5α,6α-epoxyergosta-22-en-7-one(5)、22E-ergosta-7,22-diene-3β,5α,6β-triol(6)、22E-6β-methoxyergosta-7,22-diene-3β,5α-diol(7)、22E-5α,8α-epidioxyergosta-6,22-dien-3β-ol(8)、22E-ergosta-4,6,8(14),22-tetraen-3-one(9)。结论其中化合物1是新化合物,属于5,10∶8,9二裂甾体;化合物2～9均为首次从Sporormiella属真菌中分离得到。     

南方红豆杉化学成分的分离与鉴定

目的研究南方红豆杉(Taxus chinensis var.mairei)枝叶的化学成分。方法采用反复硅胶柱色谱、ODS柱色谱、Sephadex LH-20凝胶柱色谱、高效液相制备柱色谱等方法进行分离纯化;运用现代波谱技术确定化合物的结构。结果从南方红豆杉枝叶甲醇提取物的氯仿萃取部分分离得到13个紫杉烷类化合物和1个非紫杉烷类化合物,分别鉴定为三尖杉宁碱(cephalomannine,1)、9α,10β,13α-triacetoxy-5α-cinnamoyoxytaxa-4(20),11-diene(2)、2-deacetoxytaxinine J(3)、13-cinnamoylbaccatin III(4)、7β,9α,10β,13α,20-pentaacetoxy-2α-benzoyloxy-4α,5α-dihydroxytax-11-ene(5)、2-deacetoxydecinnamoyl taxinine J(6)、Taxin B(7)、2α,7β,13α-triacetoxy-5α,10β-dihydroxy-9-keto-2(3-20)abeo-taxane(8)、taxuspine B(9)、taxachitriene A(10)、taxcuspine X(11)、7-epi-10-deacetyl taxol(12)、N-Methyltaxol C(13)、芹菜素(apigenin,14)。结论化合物6、9、12、13、14为首次从南方红豆杉(Taxus chinensis var.mairei)中分离得到,化合物7、8为首次从南方红豆杉枝叶分离得到。     

板栗种仁酸水解物化学成分的分离与鉴定

目的更好地开发利用板栗(Castanea mollissimaBlum)种仁。方法对板栗种仁的体积分数为95%的乙醇提取物进行酸水解,水解物采用硅胶柱色谱?氧化铝柱色谱、凝胶柱色谱和重结晶等方法进行分离;根据理化性质和NMR谱数据并参考文献鉴定其结构。结果分离鉴定了10个化合物,分别为对羟基苯甲酸(p-hydroxybenzoic acid,1)、原儿茶酸(protocatechuic acid,2)、没食子酸(gallic acid,3)、5-羟甲基糠醛(5-hydroxymethylfurfural,4)、β-谷甾醇(β-sitosterol,5)、α-菠甾醇(α-spinasterol,6)、齐墩果酸(oleanane acid,7)、2α-羟基齐墩果酸(maslinic acid,8)、α-香树脂醇(α-amyrin,9)、单棕榈酸甘油酯(glycerolmonopalmitate,10)。结论化合物6、8为首次从栗属植物中分离得到;化合物9为首次从板栗中分离得到。     

板栗总苞化学成分的分离与鉴定

目的分离并鉴定板栗总苞的化学成分。方法采用硅胶柱色谱、凝胶柱色谱和重结晶等多种分离方法对板栗总苞的体积分数为95%乙醇溶液回流提取物进行分离,并通过NMR和TLC等多种方法对分离得到的化合物进行结构鉴定。结果分离得到9个化合物,分别鉴定为5-羟甲基糠醛(5-(hydroxymethyl)furfural,1)、没食子酸(gallic acid,2)、对羟基苯甲酸(p-hydroxybenzoic acid,3)、对苯二酚(hydroquinone,4)、麦角甾-6,22-二烯-3β,5α,8α-三醇(ergost-6,22-diene-3β,5α,8α-tri-ol,5)、莽草酸(shikimic acid,6)、豆甾-4-烯-6β-醇-3酮(stigmast-4-en-6β-ol-3-one,7)、ganschisandrin(8)、齐墩果酸(oleanolic acid,9)。结论其中化合物6为首次从该种植物中分离得到,化合物7~9为首次从栗属植物中分离得到。     

三角叶凤毛菊化学成分研究

目的:研究三角叶凤毛菊[Saussurea deltoidea(DC.)Schulz-Bip.]化学成分。方法:利用正/反相硅胶柱色谱、Sephadex LH-20凝胶柱色谱、HPLC等方法分离化合物,运用MS和NMR等波谱方法解析鉴定化合物结构。结果:从三角叶凤毛菊中分离鉴定出9个化合物:11-hydroxy-11,13-dihydrocostol(1),6-O-(2-methylpropenoyl)-3β-hydroxy-4(15),10(14),11(13)-guaiatrien-12,8-olide(2),falbellin(3),(+)-1-hydroxypinoresinol(4),(±)-evofolin B(5),indole-3-aldehyde(6),syringaldehyde(7),loliolide(8),7-epi-loliol-ide(9)。结论:所有化合物都是首次从该植物中分离得到。     

费菜茎叶的化学成分

目的对费菜(Sedum aizoonL.)茎叶的化学成分进行研究。方法采用硅胶柱色谱?ODS柱色谱、Sephadex LH-20柱色谱和HPLC柱色谱分离纯化,依据理化性质和光谱数据确定化合物的结构。结果从费菜茎叶体积分数为70%的乙醇提取物的乙酸乙酯层中分离得到11个化合物,分别鉴定为:山柰酚(kaempferol,1)、槲皮素(quercetin,2)、杨梅素(myricetin,3)、木樨草素(luteolin,4)、山柰酚-3-O-α-L-鼠李糖苷(kaempferol-3-O-α-L-rhamnosid,5)、草质素-8-O-α-D-来苏糖苷(herbace-tin-8-O-α-D-lyxoside,6)、草质素-8-O-β-D-木糖苷(herbacetin-8-O-β-D-xylopyranoside,7)、对羟基苯酚(1,4-benzenediol,8)、没食子酸(gallic acid,9)、没食子酸甲酯(methyl gallate,10)、β-谷甾醇(β-sitostero,11)。结论化合物4、7、8为首次从该植物中分离得到,化合物5、6为首次从本属植物中得到。     

板栗种仁的化学成分(Ⅲ)

目的分离并鉴定板栗种仁的化学成分。方法采用硅胶柱色谱、凝胶柱色谱、氧化铝柱色谱和重结晶等多种分离方法对板栗种仁的95%(φ)乙醇溶液回流提取物进行分离,并通过NMR、ESI-MS和TLC等多种方法对分离得到的化合物进行结构鉴定。结果分离得到6个化合物,分别鉴定为对羟基苯甲酸(p-hydroxy benzoic acid,1),原儿茶酸(protocatechuic acid,2),没食子酸(gallicacid,3),胡萝卜苷亚油酸酯(daucosterol-6′-linoleate,4),麦角甾-6,22-二烯-3β,5α,8α-三醇(ergost-6,22-diene-3β,5α,8α-triol,5),3′,3″-di methoxylarreatricin(6)。结论其中化合物4-6为首次从栗属植物中分离得到。     

Two new sesquiterpene lactones from Sarcandra glabra

Two new sesquiterpene lactones (1) and (2), along with three known sesquiterpenes, atractylenolide beta (3), chloranthalactone E (4), and ( - )-istanbulin A (5), were isolated from the whole plant of Sarcandra glabra. The structures of two new compounds were established as 8beta,9alpha-dihydroxyeudesman-4(15),7(11)-dien-8alpha,12-olide (1) and 8beta,9alpha-dihydroxylindan-4(5),7 (11)-dien-8alpha,12-olide (2) on the basis of spectroscopic analysis. Compound 3 was isolated from this genus for the first time.     

Eremophilane sesquiterpenes from Cacalia ainsliaeflora

Chemical investigation of Cacalia ainsliaeflora afforded four new eremophilane sesquiterpenes (1 - 3, 5) and a known sesquiterpene (4), which were identified as 3 beta-angeloyloxy-8 alpha-hydroxy-6 beta-methoxyeremophil-7(11),9(10)-dien-8,12-olide (1), 3 beta-angeloyloxy-6 beta,8 alpha-dihydroxyeremophil-7(11),9(10)-dien-8,12-olide (2), 3 beta-angeloyloxy-8 alpha-hydroxy-6 beta-ethoxyeremophil-7(11),9(10)-dien-8,12-olide (3), 3 beta-angeloyloxy-8-oxo-eremphila-6,9-dien-12-oic acid (4), and 3,8-oxo-eremophila-6,9-dien-12-oic acid (5) respectively. These compounds were assayed against Escherichia coli, Staphylococcus aureus and Bacillus subtilis, and compounds 1, 2, 4 and 5 showed weak antibacterial activity. The structures of the compounds were established by 1D and 2D NMR experiments.     

Cytotoxic and ACAT-inhibitory sesquiterpene lactones from the root ofIxeris dentata formaalbiflora

Ixeris dentata forma albiflora was extracted with 80% aqueous MeOH, and the concentrated extract was partitioned with EtOAc, n-BuOH and H2O. Eight sesquiterpenes were isolated through repeated silica gel and octadecyl silica gel (C18, ODS) column chromatography of the EtOAc and n-BuOH fractions. Physicochemical analysis using NMR, MS and IR revealed the chemical structures of the sesquiterpenes, which were zaluzanin (1), 9a-hydroxyguaian-4(15),10(14),11(13)-triene-6,12-olide (2), 3beta-O-beta-D-glucopyranosyl-8beta-hydroxyguaian-4(15),10(14)-diene-6,12-olide (3), 3-O-beta-D-glucopyranosyl-8beta-hydroxyguauan-10(14)-ene-6,12-olide (4), ixerin M (5), glucozaluzanin C (6), crepiside I (7), and ixerin D (8). This is the first time that these sesquiterpene lactones have been isolated from this plant. Compounds 1, 2 and 7 revealed relatively high cytotoxicities on human colon carcinoma cell and lung adenocarcinoma cell, while compounds 5 and 7 showed acyl-CoA: cholesterol acyltransferase (ACAT) inhibitory activity.     

光果甘草三萜皂苷类化学成分研究

采用聚酰胺—大孔树脂柱色谱、ODS中压柱色谱以及半制备液相色谱分离技术,对光果甘草(Glycyrrhiza glabra L.)水提取物中三萜皂苷类成分进行分离纯化,共获得10个三萜皂苷类化合物,依据理化性质及NMR、MS波谱数据鉴定化合物结构,分别鉴定为3β-O-[β-D-glucuronpyranosyl-(1→2)-β-D-glucuronpyranosyl]-30β-O-β-Dglucuronpyranosyl-oleanane-11-oxo-12(13)-ene (1)、3β-O-[β-D-glucuronpyranosyl-(1→2)-β-D-glucuronpyranosyl]-30β-O-α-L-rhamnopyranosyl-oleanane-11-oxo-12(13)-en-22β,30-diol (2)、uralsaponin C (3)、licorice-saponin A3 (4)、licoricesaponin P2 (5)、22β-acetoxyl-glycyrrhizin (6)、macedonoside A (7)、29-hydroxyl-glycyr...     

肿节风中咖啡酸衍生物及抗氧化活性

目的对肿节风中抗氧化活性成份进行分离鉴定和抗氧化活性测定。方法利用各种色谱技术进行分离纯化,利用波谱数据鉴定结构,采用DPPH自由基清除率法测定抗氧化活性。结果从肿节风中进一步得到4个化合物,分别鉴定为:4-O-咖啡酰基-奎宁酸(4-O-caffeoylquinic acid,1),3-O-咖啡酰基-奎宁酸(3-O-caffeoylquinic acid,2),4-O-咖啡酰基-奎宁酸甲酯(4-O-caffeoylquinic acidmethyl ester,3),3-O-咖啡酰基-奎宁酸甲酯(3-O-caffeoylquinic acid methyl ester,4),各化合物显示了不同强度的抗氧化活性。结论这4个化合物均为首次从该属中分离得到,各咖啡酸衍生物、丹参素衍生物,具有邻二酚羟基的黄酮类化合物是肿节风抗氧化活性部位的物质基础。     

New eremophilane-type sesquiterpenes from Ligularia hodgsonii

Four new eremophilanlides (1- 4) together with a known sesquiterpene were isolated from the roots and rhizomes of Ligularia hodgsonii. The structures of these new compounds were established as 6beta-(2'-methylbutanoyloxy)-10beta-acetoxy-3 beta, 8beta-dihydroxyeremophil-7(11)-en-8,12-olide (1), 6beta,10 beta-dihydroxyeremophil-7(11)-en-8alpha,12-olide (2), 3beta-acetoxy-6,9-dien-8-oxoeremophil-12-nor-11-ketone (3), and 3beta-acetoxy-6alpha, 8alpha-dihydroxyeremophil-7(11), 9-dien-8,12-olide (4) by means of mass, IR and NMR spectroscopy.     

肿节风中抗氧化活性成分的研究

目的 研究中药肿节风[Sarcandra glabra (Thunb. ) Nakai.]中的抗氧化活性成分。方法 利用聚酰胺、Sephadex LH-20、Lipophilic Sephadex LH-20柱色谱以及制备型HPLC等手段进行分离,根据化合物的理化性质和波谱数据鉴定结构;采用比色法测定肿节风总多酚部位及各单体化合物对DPPH自由基的清除能力,进行抗氧化活性筛选。结果 从肿节风中分离得到2个黄酮苷类和4个有机酸类化合物,分别鉴定为朝藿定C (1)、槲皮素-3-O-鼠李糖苷 (2)、3-甲氧基-4-羟基苯甲酸 (3)、迷迭香酸-4-O-β-D-葡萄糖苷 (4)、丁香酸 (5)和对羟基苯甲酸 (6)。 结论 6个化合物均为首次从该属植物中分离得到,抗氧化活性筛选结果表明,多酚类部位为肿节风的抗氧化活性部位,化合物 2、4、5具有较强的抗氧化活性。     

New weakly cytotoxic eremophilane sesquiterpenes from the roots of Ligularia virgaurea

Six new eremophilane sesquiterpenes, including a novel nortrieremophilane carbon skeleton, were isolated from the roots of Ligularia virgaurea. Their structures were elucidated as 3 alpha,4 alpha-epoxy-6 alpha-(2'-methylacryloyl)oxy-8 alpha-methoxyeremophil-7(11)-en-8 beta,12-olide (1), 3 alpha,4 alpha-epoxy-6 alpha-(2'-methylacryloyl)oxy-8 alpha-ethoxyeremophil-7(11)-en-8 beta,12-olide (2), 1 beta,10 beta-epoxy-6 beta-(2'-methylacryloyl)oxy-8 beta-methoxyeremophil-7(11)-en-8 alpha,12-olide (3), 1 beta,10 beta-epoxy-6 beta-angeloyloxy-8 beta-methoxyeremophil-7(11)-en-8 alpha,12-olide (4), 6 beta-methoxyeremophil-7(11)-en-8 beta,12-olide (5), and 5 beta-angeloyloxy-3a,4,5,6,7,7a-hexahydro-3a beta-methyl-1 H-indene-2,4 beta-dioic acid methyl ester (6) by spectral methods, including IR, HR-ESI-MS, 1D and 2D NMR techniques. All of compounds were evaluated for their in vitro cytotoxic activities against human hepatoma (SMMC-7721), human promyelocytic leukemia (HL-60), and human hepatocyte (L-02) cells.     

HPLC法测定肿节风中异秦皮啶含量

目的测定肿节风药材中异秦皮啶含量。方法样品经甲醇加热回流提取,采用HPLC法测定。色谱柱为Alltima C18柱;流动相：乙腈-0.1%磷酸溶液（20∶80）;流速：1.0mL.min-1;检测波长：344nm。结果异秦皮啶在0.021~0.128μg范围内具有良好的线性关系（r=0.9994）;平均加样回收率（n=5）为99.4%,RSD=2.62%。结论本方法操作简便、快捷,灵敏度高,可用于肿节风中异秦皮啶的含量测定。     

Sesquiterpene lactones from Carpesium rosulatum with potential cytotoxicity against five human cancer cell lines

In search for plant-derived cytotoxicity compound against human cancer cells (A549, SK-OV-3, SK-MEL-2, XF498, HCT15), it was found that the chloroform extracts obtained from the whole plant of Carpesium rosulatum MlQ. (Compositae) exhibited significant cytotoxic activity. Four sesquiterpene lactone, CRC1 (2α, 5-epoxy-5,10-dihydroxy-6-angeloyl-oxy-9β-isobutyloxy-germacran-8α,12-olide), CRC2 (2α,5-epoxy-5,10-dihydroxy-6α,9β-diangeloyloxy-germacran-8α,12-olide), CRC3 (2α,5-epoxy-5,10-dihydroxy-6α-angeloyloxy-9β-(3-methyl-butanoyloxy)-gemacran-8α,12-olide), CRC4 (2β,5-epoxy-5,10-dihydroxy-6α,9β-diangeloyloxy-germacran-8α,12-olide) were isolated from the whole parts of C. rosulatum. 2α,5-epoxy-5,10-dihydroxy-6α,9β-diangeloyloxy-germacran-8α,12-olide (CRC2) showed the most potent cytotoxicity with IC(50) value of 6.01 μM against SK-MEL-2.