薤白的化学成分研究

目的研究薤白70%乙醇提取物的化学成分。方法采用反复硅胶柱色谱、凝胶柱色谱法进行分离纯化,根据化合物的理化性质和波谱数据鉴定化合物的结构。结果分离鉴定了6个化合物,分别为β-谷甾醇(1)、胡萝卜苷(2)、胡萝卜苷十一烷酸酯(3)、腺苷(4)、琥珀酸(5)、紫丁香苷(6)。结论其中化合物3为首次从百合科植物中分离得到。     

葛根正丁醇部位的化学成分研究

目的 研究葛根正丁醇萃取物的化学成分.方法 采用聚酰胺柱色谱、反相ODS柱色谱、凝胶柱色谱、制备液相色谱等方法进行分离纯化,根据化合物的理化性质及波谱数据鉴定其结构.结果 分离鉴定了12个化合物,分别为葛酚苷元A(1)、葛酚苷元B(2)、染料木素(3)、3′-甲氧基葛根素(4)、3′-羟基葛根素(5)、葛根素芹糖苷(6)、葛根素木糖苷(7)、大豆苷元(8)、大豆素7,4′-二葡萄糖苷(9)、大豆苷(10)、葛根素(11)、胡萝卜苷(12).结论 其中化合物1、2为首次从葛属植物中分离得到.     

黄杞叶化学成分的分离与鉴定

目的对胡桃科黄杞属植物黄杞(Engelhardtia roxburghiana Wall.)叶的水溶性部分的化学成分进行研究。方法采用硅胶柱色谱、大孔吸附树脂柱色谱、ODS柱色谱、凝胶柱色谱、制备型高效液相色谱等多种方法分离单体化合物,通过波谱数据分析鉴定结构。结果分离得到17个化合物,分别鉴定为槲皮素(quercetin,1)、山柰酚(kaempferol,2)、槲皮苷(quercitrin,3)、阿福豆苷(afzelin,4)、金丝桃苷(hyperin,5)、双氢山柰酚(dihydrokaempferol,6)、黄杞苷(engeletin,7)、异黄杞苷(isoengeletin,8)、花旗松素(taxilfolin,9)、落新妇苷(astilbin,10)、新落新妇苷(neoastilbin,11)、新异落新妇苷(neoisoastilbin,12)、异落新妇苷(isoastilbin,13)、5,7-二羟基色原酮-3-O-α-L-吡喃鼠李糖苷(eucryphin,14)、hydrojuglone glucoside(15)、juglanoside E(16)、(6S,9S)-长寿花糖苷((6S,9S)-roseoside,17)。结论化合物5、15-17为首次从黄杞属植物中分离得到。     

黄秋葵果实正丁醇部位化学成分研究

目的:对黄秋葵果实的化学成分进行研究。方法:对黄秋葵正丁醇部位采用聚酰胺柱色谱、硅胶柱色谱、ODS柱色谱、SephadexLH-20凝胶柱色谱等和制备HPLC方法分离纯化,根据其波谱数据和文献对比方法对所得化合物进行结构鉴定。结果:从黄秋葵的正丁醇部位共分离鉴定得到10个化合物,其中7个黄酮类化合物,分别是槲皮素-3-O-α-L-鼠李糖苷(1)、槲皮素-3-O-β-D-葡萄糖苷(2)、槲皮素(3)、山柰酚(5)、金丝桃苷(6)、杨梅苷(9)、橙皮苷(10);3个非黄酮类化合物为熊果酸(4)、没食子酸(7)、香草酸(8)。结论:化合物1、5-10均为首次从该植物中得到。     

马鞭草裂环环烯醚萜苷类成分的分离与鉴定

目的研究马鞭草中裂环环烯醚萜苷类成分。方法采用反复硅胶柱色谱、Sephadex LH-20柱色谱和半制备高效液相色谱等方法进行分离纯化,依据MS、1D和2D NMR(1H-1H COSY、HMQC和HMBC)进行结构鉴定。结果从马鞭草乙醇提取物的正丁醇可溶部分分离得到5个裂环环烯醚萜苷类化合物,分别鉴定为三叶草苷(trifloroside,1)、macrophylloside(2)、3′-acetylsweroside(3)、当药苦苷(swertiamarin,4)和龙胆苦苷(gentiopicroside,5)。结论化合物1~4为首次从马鞭草属植物中分离得到。     

西氏杨中防治过敏的新的酚苷

〔英〕/Ogawa Y…∥J Nat Prod.-2006,69(8).-1215~1217从西氏杨Populus sieboldii的干燥树皮中分离得到2个新的酚苷siebolside A和B(1和2),还分得3个已知化合物水杨苷(3)、樱花苷(4)和新樱花苷(5)。该植物干燥树皮依次用醋酸乙酯、70甲醇于室温提取。醋酸乙酯部位经硅胶柱色谱     

爵床中一个新的木脂体苷——爵床苷E

用硅胶柱色谱和Sephadex LH-20柱色谱对安徽产爵床(Justicia procumbens L.)全草乙醇提取物的乙酸乙酯和正丁醇部位进行分离纯化,得到6个单体化合物,通过IR、NMR等波谱技术以及一些化学方法推测化合物结构,分别为爵床脂素A(1)、新爵床脂素B(2)、爵床脂素B(3)、爵床苷B(4)、尿嘧啶(5)和爵床苷E(6),其中6为新的木脂体苷类化合物。     

四楞麻化学成分研究

为了研究土家族民间药物四楞麻的化学成分,本文采用硅胶柱色谱、凝胶柱色谱等多种柱色谱分离,制备高效液相色谱纯化,共分离得到10个单体化合物,经各种有机波谱方法鉴定化合物结构为：6″-syringyl-sesamoside (1),去咖啡酰基类叶升麻苷(decaffeoylverbascoside,2),calcelarioside B (3),类叶升麻苷(verbascoside,4),异类叶升麻苷(isoverbascoside,5),alyssonoside (6),sesamoside (7),山栀苷甲酯(shanzhiside methyl ester,8),8-乙酰山栀苷甲酯(8-acetyl-shanzhiside methyl ester,9),7-epiphlomiol (10)。其中化合物6″-syringyl-sesamoside (1)为新环烯醚萜苷类化合物,化合物2～6为首次从该植物中分离得到的苯乙醇苷类化合物。     

栀子根化学成分的分离与鉴定

目的对栀子(Gardenia jasminoides Ellis)的根进行化学成分研究。方法应用硅胶柱色谱、ODS柱色谱和Sephadex LH-20柱色谱等分离手段进行分离纯化,根据理化性质及波谱数据鉴定化合物的结构。结果从栀子根体积分数为70%的乙醇提取物中分离得到10个化合物,分别鉴定为桦木酸(betulinic acid,1)、齐墩果酸(oleanolic acid2,)、齐墩果酸-3-O-β-D-吡喃葡萄糖醛酸苷-6'-O-甲酯(oleanolic acid 3-O-β-D-glucuronopyranoside-6'-O-methyl ester,3)、常春藤皂苷元-3-O-β-D-吡喃葡萄糖醛酸苷-6'-O-甲酯(hederagenin 3-O-β-D-glucuronopyranoside-6'-O-methyl ester,4)、竹节参苷(chikusetsusaponinⅣa,5)、豆甾醇(stigmasterol,6)、β-谷甾醇(β-sitosterol,7)、胡萝卜苷(dau-costerol,8)、香草酸(vanillic acid,9)、丁香酸(syringic acid,10)。结论化合物3～5、8～10为首次从栀子属植物中分离得到,化合物12、7、为首次从栀子根中分离得到。     

箭叶淫羊藿中一个新的黄酮苷类成分

利用现代柱色谱技术,如大孔吸附树脂、硅胶、ODS、Sephadex LH-20和HW-40C柱色谱及半制备液相等对箭叶淫羊藿正丁醇部位化学成分进行分离纯化,得到14个黄酮类化合物。根据化合物的理化性质和波谱特征,确定其结构分别为3′-羟基宝藿苷-Ⅱ(1)、huazhongilexone-7-O-β-D-glucopyranoside (2)、kaempferol-3-O-α-L-rhamnoside (3)、宝藿苷-Ⅱ(4)、淫羊藿次苷-Ⅱ(5)、kaempferol 3,7-di-O-α-L-rhamnopyranoside (6)、(+)-aromadendrin (7)、kaempferol 3-O-(2-O-β-D-apiofuranosyl)-α-L-rhamnopyranoside (8)、箭藿苷A (9)、2″-O-rhamnosyl icariside-II (10)、apigenin-7-O-β-D-glucoside(11)、quercetin3-O-β-D-apiofuranoyl-(1→2)-α-L-rhamnopyranoside(12)、山柰酚(13)、淫羊...     

Comparative pharmacokinetics of equimolar doses of 5-aminosalicylate administered as oral mesalamine (Asacol) and balsalazide: a randomized, single-dose, crossover study in healthy volunteers

BACKGROUND: Existing pharmacokinetic data are insufficient to determine whether a delayed-release formulation of mesalamine (Asacol) results in greater systemic exposure to 5-aminosalicylic acid and its major metabolite N-acetyl-5-aminosalicylic acid than a prodrug (balsalazide). AIM: To determine the pharmacokinetic parameters of 5-aminosalicylic acid and N-acetyl-5-aminosalicylic acid from equimolar doses of 5-aminosalicylic acid administered as Asacol and balsalazide. METHODS: Nineteen healthy volunteers completed an open-label, single-dose, randomized, crossover study comparing the pharmacokinetics of 5-aminosalicylic acid and N-acetyl-5-aminosalicylic acid from equimolar doses of 5-aminosalicylic acid (800 mg) administered as Asacol (800 mg) and balsalazide (2250 mg). Plasma and urine samples were analysed for 5-aminosalicylic acid, N-acetyl-5-aminosalicylic acid, and balsalazide (urine only) using high-performance liquid chromatography methods with mass spectrometric detection. Pharmacokinetic parameters assessed for 5-aminosalicylic acid and N-acetyl-5-aminosalicylic acid included: percentage of dose excreted in urine (A(e)%), area under the plasma concentration-time curve (AUCt(last)); and maximum plasma concentration (C(max)). RESULTS: The geometric mean total (5-aminosalicylic acid and N-acetyl-5-aminosalicylic acid) urinary excretion values (A(e)%) of Asacol and balsalazide were 19.26 and 19.31% (P = 0.98). The geometric mean A(e)% values of 5-aminosalicylic acid for Asacol and balsalazide were 0.39 and 0.37% (P = 0.78); the geometric mean A(e)% values of N-acetyl-5-aminosalicylic acid for Asacol and balsalazide were 18.78 and 18.83% (P = 0.98). The geometric mean 5-aminosalicylic acid AUC(t(last)) values for Asacol and balsalazide were 3295 and 3449 ng h/mL (P = 0.85); the geometric mean N-acetyl-5-aminosalicylic acid AUC(t(last)) values for Asacol and balsalazide were 15 364 and 16 050 ng h/mL (P = 0.69). The geometric mean 5-5-aminosalicylic acid C(max) values for Asacol and balsalazide were 319 and 348 ng/mL (P = 0.80); the geometric mean N-acetyl-5-aminosalicylic acid C(max) values for Asacol and balsalazide 927 and 1009 ng/mL (P = 0.67). CONCLUSIONS: The systemic absorption of 5-aminosalicylic acid and N-acetyl-5-aminosalicylic acid from Asacol and balsalazide are comparable based upon plasma pharmacokinetic parameters and urinary excretion values.     

Revised structures of four saponins from Nauclea diderrichii

The interglycosidic linkages of four quinovic acid glycosides previously described from the bark of Nauclea diderrichii (de Wild) Merr. (Rubiaceae) are revised on the basis of 2D-NMR spectroscopic results. The structures were established as: quinovic acid 3-O-beta-glucopyranosyl(1-->4)-beta-fucopyranosyl-(28-->1)-beta -glucopyranosyl ester, quinovic acid 3-O-beta-glucopyranosyl-(1-->4)-alpha-rhamnopyranosyl-(28-->1)-beta-glucopyranosyl ester, quinovic acid 3-O-beta-glucopyrnaosyl-(1-->4)-beta-fucopyranoside, and quinovic acid 3-O-beta-glucopyranosyl-(1-->4)-alpha-rhamnopyranoside. The first three saponins are new compounds.     

Phenolic esters from the rhizomes of Cimicifuga racemosa do not cause proliferation effects in MCF-7 cells

Five phenylpropanoid esters, caffeoylglycolic acid, 2-caffeoylpiscidic acid (cimicifugic acid D), 3,4-dihydroxyphenacyl caffeate (petasiphenone), 3,4-dihydroxyphenyl-2-oxopropyl isoferulate (cimiciphenol) and 3,4-dihydroxyphenacyl isoferulate (cimiciphenone) were isolated from a commercially available extract of the rhizomes of Cimicifuga racemosa (L.) Nutt. (syn. Actaea racemosa L.) for the first time; the known cimicifugic acids A, B, E, F, fukinolic acid, fukiic acid and caffeic acid were also obtained. Cimiciphenone and caffeoylglycolic acid are new natural products. The structures were elucidated by means of spectroscopic data (ESI-MS, 1H-, 13C-NMR, COSY, HMQC, HMBC and NOE experiments). Ferulic acid and isoferulic acid were detected by HPLC analysis in comparison to standards. The estrogenic activity of the isolated compounds was tested in an estrogen-dependent MCF-7 mamma carcinoma cell line; 17beta-estradiol (10(-11) M) and the phytoestrogen coumestrol (10(-7) - 10(-5) M) were used as references. The results suggest that, in contrast to an earlier report, the phenolic esters do not exert a proliferative (estrogenic) effect in this test system.     

紫珠果实中脂肪酸的GC-MS分析

目的：研究紫珠果实中脂肪酸成分,方法：采用GC－MS技术。结果：从紫珠果实中分离得7个脂肪酸、并测定了相对含量,鉴定出紫珠果实中含棕榈酸（11．37％）、亚油酸（64．5％）、油酸（17．2％）、硬脂酸（4．62％）、花生二烯酸（6．65％）,花生三烯酸（0．41％）、花生酸（0．7％）。结论：以上化合物均首次从该植物中分离鉴定。     

Metabolites of (+)-dehydroabietic acid in rabbits

The seven metabolites of (+)-dehydroabietic acid (DHA) were newly isolated from rabbit urine by liquid chromatography. On the basis of chemical and spectral data their structures were established to be (15S)-8,11.13-abietatrien-16,18-dioic acid, 2 alpha-hydroxy-8,11,13,15-abietatetraen-18-oic acid, (15R)-15,16-dihydroxy-8,11,13-abietatrien-18-oic acid, 2 beta,15-dihydroxy-8,11,13-abietatrien-18-oic acid, (15S)-2 beta,16-dihydroxy-8,11,13-abietatrien-18-oic acid, 2 alpha,15-dihydroxy-8,11,13-abietatrien-18-oic acid, and (15S)-2 alpha,16-dihydroxy-8,11,13-abietatrien-18-oic acid. The possible hydroxylation routes of DHA in rabbits and the difference between the metabolism of DHA in microorganisms and that in rabbits are discussed.     

野西瓜果皮中有机酸类化学成分的分离与鉴定

目的研究野西瓜(Capparis spinosa L.)果皮中有机酸类化学成分,为进一步阐明其抗炎抗菌活性成分、充分开发利用提供科学依据。方法采用硅胶柱色谱、羟丙基葡聚糖凝胶柱色谱等方法进行分离纯化,并通过理化常数测定和波谱分析鉴定其化学结构。结果从野西瓜果皮中分离得到了6个有机酸类化合物,即香草酸(vanillic acid,1)、4-羟基苯甲酸(4-hydroxybenzoic acid,2)、原儿茶酸(protocatechuic acid,3)、2,4-二羟基苯甲酸(2,4-dihydroxybenzoic acid,4)、丁二酸(succinic acid,5)、邻苯二甲酸二(2-乙基)己酯(bis(2-ethylhexyl)phthalate,6);分离得到3个甾体类化合物为β-谷甾醇(β-sitosterol,7)、胡萝卜苷(daucosterol,8)、α-菠菜甾醇-3-O-β-D-吡喃葡萄糖苷(α-spinasterol-3-O-β-D-glucopyranoside,9)。结论化合物4、6、9为首次从山柑属植物中分离得到。     

Polynucleotide analogues. Copolymers of vinyl bases with acrylic acid, methylacrylic acid, acrylamide, and 1-vinylpyrrolidone.

Preliminary studies are reported on the synthesis and testing of substituted vinyl polymers that are designed to have sequence specific affinity for polyribonucleic acids. Copolymers of 1-vinyluracil with acrylic acid, 2-methylacrylic acid, or 1-vinyl-2-pyrrolidone were prepared by gamma-irradiation to give the respective polymers 1,3, and 4. Similarly, 9-vinyladenine yielded copolymeric products 5 and 6 with acrylic acid or 2-methylacrylic acid. Radical initiated polymerization of 9-vinyladenine with acrylamide yielded copolymer 7. The products were characterized by elemental analysis and ultraviolet, infrared, and nuclear magnetic resonance spectroscopy. No hypochromicity could be detected on mixing polymers 1-4 with poly(adenylic acid). The acrylic acid copolymer 2 containing a high ratio of vinyluracil was a potent inhibitor of poly(adenylic acid) coded polylysine synthesis in an in vitro system. Polymers 6 and 7, containing a high proportion of vinyladenine, inhibited poly(uridylic acid) coded poly(phenylalanine) synthesis.     

Hydroxycinnamic Acid Derivatives Obtained from a Commercial Crataegus Extract and from Authentic Crataegus spp.

Eleven hydroxycinnamic acid derivatives were isolated from a 70% methanolic Crataegus extract (Crataegi folium cum flore) and partly verified and quantified for individual Crataegus species (C. laevigata, C. monogyna, C. nigra, C. pentagyna) by HPLC: 3-O-(E)-p-coumaroylquinic acid (1), 5-O-(E)-p-coumaroyl-quinic acid (2), 4-O-(E)-p-coumaroylquinic acid (3), 3-O-(E)-caffeoylquinic acid (4), 4-O-(E)-caffeoylquinic acid (5), 5-O-(E)-caffeoylquinic acid (6), 3,5-di-O-(E)-caffeoylquinic acid (7), 4,5-di-O-(E)-caffeoylquinic acid (8), (-)-2-O-(E)-caffeoyl-L-threonic acid (9), (-)-4-O-(E)-caffeoyl-L-threonic acid (10), and (-)-4-O-(E)-p-coumaroyl-L-threonic acid (11). Further, (-)-2-O-(E)-caffeoyl-D-malic acid (12) was isolated from C. submollis and also identified for C. pentagyna and C. nigra by co-chromatography. The isolates 10 and 11 were not found in the authentic fresh specimen, indicating that they may be formed during extraction by acyl migration from the 2-O-acylderivatives. Also, 9 and 11 are described here for the first time. All structures were assigned on the basis of their spectroscopic data (¹H-, ¹³C-NMR, MS, optical rotation).     

豨莶脂溶性成分的研究

从豨莶(Siegesbeckia orientalis L.)的地上部分,分离出八个化合物,其中I和I根据理化性质和光谱数据确定其结构为ent-17-acetoxy-18-isobutyryloxy-16(α)-kauran-19-oicacid(I)和ent-17-ethoxy-16(α)-kauran-19-oicacid(II),均为新化合物,分别被命为豨莶酯酸(siegesesteric acid,I)和豨莶醚酸(siegesetheric acid,I)。其余化合物分别鉴定为腺梗豨莶萜醇酸(ent-16β,17-dihydroxy-kauran-19-oicacid,II),奇任醇(kirenol,IV,β-谷甾醇葡萄糖甙(β-sitosterolglucoside,V),二十一醇(heneicosanol,VI),花生酸甲酯(methyl arachidate,VII)和β-谷甾醇(β-sitosterol,VII)。除奇任醇和β-谷甾醇外,均为首次从该植物中分得。