夏枯草皂苷A的结构鉴定

目的：研究夏枯草(Prunella vulgaris L.)果穗中的化学成分。方法：用色谱法分离夏枯草的化学成分,并用化学及波谱法鉴定其结构。结果：从夏枯草中分离得到6个化合物,根据理化性质和波谱数据鉴定其结构分别为β-香树脂醇（1）,α-波甾醇（2）,豆甾醇（3）,豆甾-7-烯-3β-醇（4）,咖啡酸（5）和2α,3α,24-三羟基-齐墩果-12-烯-28-酸-28-β-D-吡喃葡糖酯苷（6）。并将其亲脂性部分甲基化后用气质联用方法进行分析,从中分离鉴定了8个脂肪酸类化合物。 结论：化合物6为新化合物,命名为夏枯草皂苷A,化合物2～5为首次从夏枯草获得。     

楝树皮中的四环三萜类化合物

楝科植物楝树（Melia azedarach L.）为中药苦楝皮的基源植物之一。本研究从楝树的干燥树皮中分离鉴定出了8个化合物：其中6个为四环三萜类化合物,分别为meliastatin 3（1）、dubione B（2）、toosendanone A（3）、sendanolactone（4）、melianodiol（5）和1-tigloyl-3,20-diacetyl-11-methoxymeliacarpinin（6）;2个为甾醇类化合物,即豆甾-5-烯-3β,7α-二醇（7）和豆甾-4-烯-3β,6β-二醇（8）。化合物7、8为首次从楝属植物中分离得到,化合物1、2、3为首次从楝树中分离得到,化合物4、5、6为首次从楝树树皮中分离得到。     

海洋真菌Rhizopus sp.菌丝体中化学成分的研究

目的对海洋真菌Rhizopus sp.菌丝体的丙酮和甲醇萃取部分进行化学成分的研究.方法采用硅胶柱色谱、凝胶柱色谱、高效液相色谱等手段,利用理化和波谱分析方法,对海洋真菌Rhizopus sp.菌丝体中的化合物进行分离鉴定.结果与结论从该真菌菌丝体中分离得到6个化合物.经光谱数据分析,鉴定其结构为5α,8α-过氧麦角甾-6,22-二烯-3β-醇(1)、1-O-9(Z)-十八碳烯酰甘油酯(2)、麦角甾-7,22-二烯-3β,5α,6β-三醇(3)、麦角甾-8(9),22-二烯-3β,5α,6β,7α-四醇(4)、戊五醇(5)、尿素(6).这些化合物均为首次从该真菌菌丝体中分离得到.     

长毛囊孔菌发酵液化学成分研究

目的研究长毛囊孔菌（Trametes versatillis. Berk）液体深层发酵产生次生代谢产物。方法利用常规色谱分离技术对长毛囊孔菌发酵液和菌丝体的提取物进行分离。结果分离鉴定了7个化合物,经波谱分析分别鉴定为D-阿洛醇（1）、3β-羟基-麦角甾-5,7,22-三烯（2）、3β-羟基-5α,8α-过氧化麦角甾-6,22-二烯（3）、eburicoic acid（4）、3β-羟基-5α,8α-过氧麦角甾-6,22-二烯（5）、tumulosic acid（6）和软脂酸-α-甘油酯（7）。结论以上化合物都为长毛囊孔菌中首次报道,且三萜化合物在长毛囊孔菌发酵液及发酵菌丝中含量较大,具有一定的深入研究价值。     

虎眼万年青的化学成分

目的：研究栽培于长白山区的虎眼万年青Ornithogalum caudatum Ait全草的化学成分。 方法：用各种色谱技术进行分离和纯化,用ESIMS,IR,¹HNMR,¹³CNMR,DEPT,¹H-¹H COSY, ¹H-¹³C COSY, HMBC和NOESY等波谱数据分析鉴定结构。结果：从虎眼万年青全草中分离得到3个化合物,其中化合物I为新化合物,其结构鉴定为（25S, 23S, 24S）-螺甾-Δ⁵⁽⁶⁾-烯-1β, 3β,23,24-四醇-1-O-α-L-吡喃鼠李糖基-（1→2） ［β-D-吡喃木糖基-(1→3)］-α-L-吡喃阿拉伯糖苷(I),另外2个已知化合物为海柯皂苷元-3-O-{β- D-吡喃葡糖基（1→2）-［β-D-吡喃木糖基（1→3）］-β-D-吡喃葡糖基（1→4）-β-D-吡喃半乳糖苷}(II)和β-谷甾醇(III)。结论：化合物I为新化合物,命名为虎眼万年青苷A,化合物II和III是首次从该植物中分得的已知化合物。     

无纹紫背苔化学成分的研究

目的　研究苔纲植物无纹紫背苔（Plagiochasm intermedium L.）的化学成分。方法　用95%的EtOH回流提取,所得浸膏分部萃取后经硅胶柱及Sephadex LH-20柱色谱反复分离纯化,并用1DNMR,2DNMR及X-ray单晶衍射等技术对化合物的结构进行鉴定。 结果　从无纹紫背苔中分离到6个化合物,分别鉴定为：双联苄类化合物Pakyonol（I）, 24-乙基胆甾-5,22-二烯-3β-软脂酸脂（24-ethylcholesta-5,22-dien-3β-ol-palmitic acid ester,II）, 22-羟基何伯烷（22-hopanol,III）, β-谷甾醇（β-sitosterol, IV）,胡萝卜苷（daucosterol,V）,甘露醇（mannitol,VI）。 结论　II为新化合物, 其余化合物为首次从该属植物中分离得到。     

海燕化学成分研究

目的：研究海燕的化学成分。方法：采用多种层析方法分离海燕乙醇提取物,根据理化性质和光谱数据分析鉴定化合物的结构。结果：分离鉴定了7个化合物,分别为：3-十八烷氧基-1,2丙二醇（1）,3β-羟基-胆甾-7烯（2）,asterosaponin P1（3）,5α-胆甾烷-3β,4β,6α,7α,8β,15β,16β,26-八醇（4）,5α-胆甾烷-3β,6α,7α,8β,15α,16β,26-七醇（5）,色氨酸（6）,苯丙氨酸（7）。结论：化合物1、2为首次从海燕中分离得到,化合物4为首次从中国海域的海燕中分离得到。     

一株产生苝醌类化合物真菌的化学成分研究

目的研究菌寄生菌属真菌（Hypomyces (Fr.) Tul. sp.）菌丝体的化学成分。方法用硅胶柱色谱法进行分离纯化，根据理化性质和光谱数据进行结构鉴定。结果从菌丝体中分得两个化合物，命名为hypomycin C（I）和hypomycin D（II)。结论I和II均为新化合物。     

海洋真菌96F197抗癌活性成分研究

目的对海洋真菌代谢产物中抗癌活性成分进行分离和结构鉴定,并对得到的化合物进行体外抗癌活性评价。方法用硅胶、SephedaxHL-20、ODS柱色谱及制备高效液相色谱等方法进行分离,通过化合物的理化性质及各种光谱技术鉴定化合物的结构。采用MTT法测定化合物体外抗癌活性。结果从真菌菌丝体的丙酮提取物中分离得到两个生物碱类化合物和两个甾醇类化合物,分别鉴定为viridicatol(1)、sclerotiamide(2)、22E-5α,6α-环氧麦角甾-8(14),22-二烯-3β,7α-二醇(3)、22E-5α,8α-桥二氧麦角甾-6,22-二烯-3β-醇(4)。化合物3和4在50μg·mL-1的质量浓度下可以明显地抑制HepG2、人乳腺癌MCF-7细胞和NCI-H460肿瘤细胞的生长。结论化合物3和4有明显的体外抗癌作用。     

芫花花蕾中甾醇类化合物的分离与鉴定

目的对瑞香科瑞香属植物芫花(Daphne genkwa Sieb.et Zucc.)花蕾中的甾醇类化学成分进行分离与结构鉴定。方法运用硅胶﹑Sephadex LH-20柱色谱﹑重结晶等分离手段进行甾醇类化合物的分离纯化,根据理化性质及波谱数据鉴定其化学结构。结果从芫花花蕾的体积分数95%乙醇提取物中分离得到6个化合物,分别鉴定为:豆甾-5-烯-3β,7α-二醇(stigmasta-5-ene-3β,7α-diol,1)、豆甾-5-烯-3β,7β-二醇(stigmasta-5-ene-3β,7β-diol,2)、豆甾-4-烯-3β,6β-二醇(stigmasta-4-ene-3β,6β-diol,3)、7-ketositosterol(3β-hydroxysitost-5-ene-7-one,4)、过氧化麦角固醇(ergosterol peroxide,5)和β谷甾醇-3β-吡喃葡萄糖苷-6'-O-棕榈酸酯(β-sitosteryl-3β-glucopyranoside-6'-O-palmitate,6)。结论化合物2⁶为首次从瑞香属植物中分离得到,化合物1为首次从芫花植物中分离得到。     

大叶茜草化学成分的研究

自大叶茜草Rubia schumanniana Pritz的根中分离到五种化学成分,其中一个经光谱及化学方法测定,证明结构为3′-甲氧羰基-4′-羟基-6,6-二甲基萘骈(1′,2′-2,3)吡喃,是新化合物,命名为大叶茜草素(rubimaillin)。另外四个为已知成分,其中三个为蒽醌类化合物,分别鉴定为1-羟基-2-羟甲基蒽醌,1-羟基-2-甲基蒽醌及1,4-二羟基-2-甲基蒽醌,另一为β-谷甾醇。     

狭叶香蒲花粉(蒲黄)黄酮类成分的研究

自香蒲科(Typhaceae)植物狭叶香蒲(Typha augustifolia L.)的干燥花粉中分离到五个黄酮醇甙,包括两个黄酮醇-3-三糖甙(Ⅰ,Ⅱ)和三个黄酮醇-3-双糖甙(Ⅲ,Ⅳ,Ⅴ)。其中,化合物Ⅰ是一个新的黄酮醇甙,为本植物的主要成分,经光谱分析(UV,IR.MS;¹HNMR和¹³CNMR)和水解试验确定为异鼠李素-3-0-(2_G-α-L-鼠李糖基)-α-L-鼠李糖(1→6)-β-D-葡萄糖甙,命名为香蒲新甙(typhaneoside,Ⅰ)。其它四种为已知成分。Ⅱ从本属植物中首次发现。     

A novel indole alkaloid from deep-sea sediment metagenomic clone-derived Escherichia coli fermentation broth

To explore secondary metabolites in deep-sea sediment metagenomic clone-derived Escherichia coli fermentation broth, different kinds of chromatography methods were used in the isolation procedures, while the structures of the isolated compounds were assigned based on the MS analysis and their ¹H and ¹³C NMR spectra including 2D NMR techniques such as COSY, HMQC, and HMBC experiments. As a result, a novel compound was isolated and characterized as N-{1-[4-(acetylamino)phenyl]-3-hydroxy-1-(1H-indol-3-yl)propan-2-yl}-2,2-dichloroacetamide (1). In addition, eight known compounds were also obtained. Fatty acid amide hydrolase and monoacylglycerol lipase were used to screen analgesic activity, and the new compound showed analgesic activity to some extent in pharmacological test.     

A new antibacterial compound from Luo Han Kuo fruit extract (Siraitia grosvenori)

Luo Han Kuo fruit (Siraitia grosvenori Swingle) has been used in China for centuries as a sweetening agent, and also used to treat sore throat and cough. In our recent study, a new bioactive compound, (2R,3S,4S)-2,3-trans-3,4-cis-5,3′-bimethoxy-7-(trans-2-propenal)-3,4-flavandiol (1), named siraitiflavandiol was obtained. The structure has been determined on the basis of spectroscopic studies including 1D and 2D NMR (¹H, ¹³C NMR, ¹H–¹H COSY, HSQC, HMBC, and NOESY), CD, EI-MS, and HR-EI-MS spectra. The new compound was evaluated in vitro for its inhibitory ability against the growth of oral bacterial species Streptococcus mutans, Porphyromonas gingivalis, and yeast Candida albicans. The minimum inhibitory concentrations were 6, 24, and 6 μg/ml, respectively.     

Radiosynthesis and in vitro evaluation of 1‐(tetrahydro‐5‐hydroxy‐6‐(hydroxymethyl)‐2H‐pyran‐3‐yl)‐5‐[125I]iodouracil: A new potential agent for HSV1‐tk reporter gene monitoring

Synthesis, radiolabelling, and in vitro evaluation of a new ¹²⁵I‐labelled iodouracil hexitol nucleoside analogue are reported. The target compound was successfully synthesized by an iodination–destannylation method and then purified by reverse phase HPLC. The radiochemical purity of the product was >99% with decay‐corrected yields of 48±3%. In vitro cellular uptake testing was carried out using MCA and MCA‐tk cell lines for comparison of compound 1 with [¹⁸F]FHBG. The newly synthesized compound 1 showed higher accumulation in herpex simplex virus type 1 thymidine kinase (HSV1‐tk) gene expression cell line (MCA‐tk cell line) than in the wild type MCA cell line compared with [¹⁸F]FHBG. The MCA‐tk to MCA cellular uptake ratio for compound 1 was higher than that of [¹⁸F]FHBG from 2 h after incubation. The radioiodine‐labelled compound 1 (I‐125, t_1/2=59.37 days) has a longer physical half‐life than F‐18‐(t_1/2=110 min) labelled FHBG. Radioiodine‐labelled compound 1 could be used for monitoring gene expression for a long time. The selectivity for MCA‐tk cell line makes compound 1 a promising imaging agent for HSV1‐tk expression. Copyright © 2010 John Wiley & Sons, Ltd.     

Asterosaponins and glycosylated polyhydroxysteroids from the starfish Culcita novaeguineae and their cytotoxic activities

Using combined chromatographic methods, two asterosaponins (compounds 1 and 2), including a new compound novaeguinoside E (compound 1), and six glycosylated polyhydroxysteroids (compounds 3–8) were isolated from a methanol extract of the starfish Culcita novaeguineae. Their structures were determined on the basis of spectroscopic data (¹H and ¹³C NMR, HSQC, HMBC, ¹H–¹H COSY, ROESY, and HRESI-MS) and by comparison with the literature values. The new compound 1 represents the third example of asterosaponins containing the 5α-cholesta-9(1l)-en-3β,6α,20,22-tetraol aglycone. Among isolated compounds, 4–7 exhibited moderate to weak cytotoxic activities against five human cancer cell lines such as Hep-G2 (hepatoma), KB (epidermoid carcinoma), LNCaP (prostate cancer), MCF7 (breast cancer), and SK-Mel2 (melanoma).     

鼓槌石斛化学成分的研究

自中药鼓槌石斛(Dendrobium chrysotoxum Lindl.)茎中分离到5个化合物,经光谱(UV,IR,MS,¹HNMR,DIFNOE和¹³CNMR)分析,分别鉴定为β-谷甾醇(I)、鼓槌菲(chrysotoxene,II)、毛兰素(erianin,III)、毛兰菲(confusarin,IV)和鼓槌联苄(chrysotobibenzyl,V)。II是新化合物,V是新天然产物。     

甘草叶中甘草宁P-3′-甲醚的分离和鉴定

Two flavonoids were isolated from the leaves of Glycyrrhiza uralensis Fisch (Licorice, Leguminosae). On the basis of physico-chemical properties and spectroscopy (UV, ¹HNMR and MS), a new compound was elucidated as 3,5,7,4′-tetrahydroxy-3′-methoxy- 6-isoprenyl flavone (gancaonin P-3′-methylether) and another known compound was identified as 8-C-prenyleriodictyol.     

Isolation and characterization of a new anticancer diterpenoid from Jatropha gossypifolia

Jatropha gossypifolia root bark is used in ethnomedicine for the treatment of various diseases and infections. We have studied the phytochemistry and evaluated the anticancer activity of J. gossypifolia root extract. Phytochemical investigation of the root of J. gossypifolia resulted in the isolation and characterization of one new diterpenoid along with four well-known compounds. The new compound was established by 1D and 2D NMR spectra and x-ray analysis, while spectral (¹H, ¹³C NMR, and ESI-MS) characteristics of the known compounds were compared with reported data. The new compound showed potent proliferation inhibitory activity against A-549 human cancer cell line.     

Scyphiphin D,a new iridoid glucoside dimer from Scyphiphora hydrophyllacea

From the aerial parts of Scyphiphora hydrophyllacea Gaertn. F., a new iridoid glucoside dimer scyphiphin D (1) and a known iridoid glucoside geniposidic acid (2) were isolated. The structure of this new compound was determined on the basis of HR-FAB-MS, IR, ¹H and ¹³C NMR (DEPT), and 2D NMR (HMQC, HMBC, COSY, ROESY) spectral data.