新月菱形藻胞外多糖的成分及其硫酸酯的制备

目的阐明新月菱形藻胞外多糖(exopolysaccharides of Nitzschia closterium,EPN)的成分、单糖组成及其硫酸酯化条件。方法新月菱形藻胞外多糖以醇沉法从该藻的培养液中制备;DEAE-Sephedex25柱分离,HPLC法测定其质量分数,HPLC测定其相对分子质量;以氯磺酸-吡啶法探索新月菱形藻硫酸酯化反应条件。结果新月菱形藻向胞外分泌3种多糖,相对分子质量分别为EPN11.886×105,EPN21.41×105,EPN31.134×105。3种多糖的单糖组成均为甘露糖、鼠李糖、葡萄糖醛酸、葡萄糖和岩藻糖。甘露糖、鼠李糖、葡萄糖醛酸、葡萄糖和岩藻糖的摩尔比在EPN1为4.3∶1∶5.1∶8.9∶5.6,EPN2为4.2∶7.3∶3.7∶12.8∶3.4,EPN3为3.5∶2.1∶4.3∶4.9∶4.7。3种多糖的硫酸酯化条件基本一致,提高氯磺酸比例和延长反应时间均有利于增加酯化产物的硫酸根、提高取代度和酸酯化反应的产率。结论新月菱形藻胞外多糖为酸性多糖,其硫酸酯化产物多糖硫酸酯可能具有潜在的药理活性。     

千年健化学成分研究(Ⅱ)

目的:对广西产千年健Homalom ena occulta(Lour.)Schott的化学成分进行系统研究。方法:运用多种柱层析分离手段进行了单体化合物的分离,通过波谱技术及理化数据确定化合物的结构。结果:从石油醚和正丁醇部位共分离并鉴定了6个化合物。其中包括石油醚部位的三个化合物,分别为:α-羟基二十五碳酸(α-Hydroxypentacosanoic ac id 1),棕榈酸(Palm itic ac id2)及十五碳酸(Pentadecanoic3)和正丁醇部位的三个化合物,它们分别为:葡萄糖(G lucose4),D半-乳糖醇(D-galac ititol5)及赤鲜醇(Erythritol6)。结论:此六个化合物均为首次从该种植物中分离得到。其中化合物1为首次从自然界中分离得到。     

人参皂苷M1异丁酸酯衍生物的合成及高效液相分析和制备

目的：研究人参皂苷M1异丁酸酯合成过程中产物的高效液相分析及快速制备方法。方法：采用保护-酯化-去保护的方法,定向修饰得到M1糖基3 位酯化的产物;利用反相高效液相色谱,采用DAD检测器,通过对分析条件的优化,建立人参皂苷M1异丁酸酯及其两个中间产物的分析制备方法。结果：人参皂苷M1异丁酸酯及其中间产物的分析和制备时间均在40 min以内快速高效地获得;综合三步反应和高效液相制备结果,合成人参皂苷M1异丁酸酯的得率为367%,纯度为983%。结论：采用HPLC法,在M1衍生物合成过程中可以快速高效地进行人参皂苷M1衍生物的分析和制备。     

鹰嘴豆中三种异黄酮酯化反应研究

目的:改善鹰嘴豆中3种异黄酮的药物活性。方法:以鹰嘴豆芽素A、刺芒柄花素、染料木素为原料,对其进行4-溴丁酰酯化反应、EDC缩合反应、正丁酰酯化反应。结果:合成了12个异黄酮类衍生物,方法简单、条件易控、产率较高。结论:产物结构通过1H-NMR、13C-NMR、ESI-MS分析确认,为进一步对其药物活性研究奠定结构基础。     

药用植物种子的植物化学研究Ⅱ:桔梗种子中一种新的二氢黄酮醇糖甙和一种新的3-甲基-1-丁醇糖甙

从桔梗(Platycodon grandiflorum)的种子中分离出2种新的糖甙,分别命名为flavoplatycoside(1)和grandoside(2)。根据化学和光谱数据确定它们的化学结构分别为(2R,3R)-黄杉素7-O-α-L-吡喃鼠李糖基-(1→6)-β-D-吡喃葡萄糖甙和3-甲基-1-丁醇1-O-β-D-吡喃葡萄糖基-(1→2)-β-D-吡喃葡萄糖甙。同时还分离出4     

中乌头碱的丙酰化修饰研究

目的 探讨中乌头碱C_3,C_(13),C_(15)位羟基的丙酰化方法.方法 以中乌头碱、丙酸酐为原料合成中乌头碱酯化衍生物.结果 得到4种丙酰化衍生物,并通过ESI-MS,1H-NMR验证了其结构,分别为3-丙酰基中乌头碱(a);3,13,15-三丙酰基中乌头碱(b);3-丙酰基-13,15-二乙酰基中乌头碱(c);3-乙酰基-13 -丙酰基中乌头碱(d).据文献检索,所有化合物均为首次报道. 结论中乌头碱的三个羟基中,C_3-OH最易被丙酰化,C_(15)-OH最难被丙酰化.     

黄荆中的三种新黄酮甙

本文报告从黄荆(Vitex negundo)中分得三种新黄酮化合物A、B、C。化合物-A(I),mp>300°,200°分解,C_(32)H_(40)O_(17)·H_2O,红外光谱v_(max)~(KBr)cm~(-1):3340(OH)、288.5(OCH_3)、1667(共轭羰基)。紫卜光谱。λ_(max)~(MeOH)253nm、273nm和340nm,显示黄酮骨架,C-3取代黄酮的定性反应呈阳性。三氯化铝处理后吸收峰不向长波方向移动,表明C_5-OH和C_3-OH被取代。酸水解后得到了葡萄糖和鼠李糖。甙元     

鹰嘴豆中三种异黄酮结构修饰衍生物的合成及其结构表征

目的:改善鹰嘴豆中三种异黄酮的溶解性,提高其生物利用度。方法:以刺芒柄花素、鹰嘴豆芽素A、染料木素为原料,对其进行异丁基化反应、异丁酰酯化反应、苯磺酰酯化反应。结果:合成了10个异黄酮类衍生物,方法简便、条件易控、产率较高。结论:产物结构通过1H-NMR、13C-NMR、ESI-MS分析确认,为进一步对其生物活性研究奠定结构基础。     

聚乙二醇化葛根素化学结构初步鉴定

采用紫外、红外、氢核磁、碳核磁光谱联用技术对聚乙二醇(PEG)化葛根素的化学结构进行初步鉴定,结果推测2个PEG高分子(分子量:4700 Da)分别与葛根素葡萄糖基上的3″-OH和6″-OH仲羟基酯键结合。首次采用光谱联用技术对PEG高分子修饰物进行化学结构的初步鉴定。     

狗脊中新的水溶性鞣质

目的:深入研究狗脊中的化学成分.方法:采用柱色谱和高效液相色谱法分离纯化狗脊中的化学成分,并采用质谱和核磁共振技术鉴定其结构.结果:1个新的酚性成分,即4-O-咖啡酰-D-葡萄糖被分离得到,其结构通过1D,2D NMR和ESI-MS鉴定.结论:4-O-咖啡酰-D-葡萄糖首次从狗脊中分离得到,该化合物为新的酚性化合物.     

一个新颖的人参皂苷元衍生物及其抗HL-60肿瘤细胞活性

目的研究人参皂苷元衍生物及其抗HL-60肿瘤细胞活性。方法利用Smith降解处理人参总皂苷,采用硅胶柱色谱、制备型高效液相色谱技术分离、纯化人参皂苷元等产物。通过波谱数据分析产物结构。采用MTT法测试产物抗HL-60肿瘤细胞活性。结果分离鉴定了原人参二醇(PD)、原人参三醇(PT)和24,25-烯-3β,6α-二羟基-12,20-(1′-羟基)双氧乙基-达玛烷(1),化合物1为新化合物命名为1′-羟基双氧乙基原人参三醇。结论化合物1为新型人参皂苷元衍生物,其抑制HL-60细胞增殖的作用强于PD和PT。     

褐藻叉开网翼藻化学成分研究

目的:对网地藻科褐藻叉开网翼藻进行化学成分研究,并对分离得到的化合物进行细胞毒活性实验。方法:利用正相硅胶柱色谱、Sephadex LH-20柱色谱、反相HPLC及重结晶等手段进行分离纯化;借助IR,MS及NMR鉴定结构;通过改良的MTT法对单体化合物进行细胞毒活性实验。结果:从叉开网翼藻中分离得到8个化合物,分别鉴定为(-)-torreyol(Ⅰ),4β,5-αdihydroxycubenol(Ⅱ),3-farnesyl--phydroxybenzioc acid(Ⅲ),chromazonarol(Ⅳ),岩藻甾醇(Ⅴ),苯乙酰胺(Ⅵ),4-羟基苯甲酸(Ⅶ)和正十六酸(Ⅷ)。结论:化合物Ⅱ和Ⅳ系首次从该海藻中发现;其余化合物均为首次从网地藻科海藻中分离得到。细胞毒活性试验结果显示所有化合物均无明显活性(IC50>10μgmL-1)。     

A New Triterpenoid Saponin from Aidi Injection

Objective To investigate the chemical constituents from Aidi Injection.Methods The chemical constituents were isolated by chromatography on Sephadex LH-20 gel columns and reverse phase semi-preparative HPLC repeatedly.Their structures were identified by spectroscopic analysis(NMR and MS).Results Twenty-two compounds were isolated and identified to be 3-O-3′,4′-diacetyl-β-D-xylopyranosyl-6-O-β-D-glucopyranosyl- cycloastragenol(1),astragaloside IV(2),astragaloside II(3),astragaloside I(4),isoastragaloside I(5), acetylastragaloside I(6),ginsenosid Re(7),ginsenoside Rf(8),ginsenoside Rg1(9),ginsenoside Rb3(10), notoginsenoside R4(11),ginsenoside Rb1(12),ginsenoside Rc(13),ginsenoside Rb2(14),ginsenoside Rd(15), lucyoside H(16),3-O-β-D-glucopyranosyl(1→4)-β-D-glucopyranosyl(1→3)-α-L-rhamnopyranosyl(1→2)-α-L- arabinopyranosyl oleanolic acid 28-O-α-L-rhamnopyranosyl(1→4)-β-D-glucopyranosyl(1→6)-β-D-glucopyranoside (17),3-O-β-D-glucopyranosyl(1→3)-α-L-rhamnopyranosyl[β-D-glucopyranosyl-(1→4)]-(1→2)-α-L-arabinopyranosyl oleanolic acid 28-O-α-L-arabinopyranosyl(1→4)-β-D-glucopyranosyl(1→6)-β-D-glucopyranoside(18),syringin (19),elentheroside E(20),4-(1,2,3-trihydroxypropyl)-2,6-dimethoxyphenyl-1-O-β-D-glucopyranoside(21),and coniferin(22).Conclusion Compounds 1-6 are originated from Astragalus membranceus,compounds 7-18 are originated from Panax ginseng,and compounds 19-22 are originated from Acanthopanax senticosus by LC-MS analysis.Compound 1 is a new compound.     

Izumiphenazines A-C: isolation and structure elucidation of phenazine derivatives from Streptomyces sp. IFM 11204

Three new phenazine derivatives, named izumiphenazines A-C (1-3), and the known phenazine-1,6-dicarboxylic acid (4) were isolated from Streptomyces sp. IFM 11204. The structures of the isolated compounds were elucidated by means of spectroscopic methods including UV, IR, HRESIMS, and 1D and 2D NMR. Compounds 1-3 were evaluated for their activity in overcoming TRAIL (TNF-related apoptosis-inducing ligand) resistance in human gastric adenocarcinoma cells. Compounds 2 (30 μM) and 3 (20 μM) in combination with TRAIL showed synergistic activity in sensitizing TRAIL-resistant AGS cells.     

Steroids and flavonoids from Physalis alkekengi var. franchetii and their inhibitory effects on nitric oxide production

Four new steroidal compounds possessing a rare 13,14-seco-16,24-cycloergostane skeleton, physalin Y ( 1), physalin Z ( 2), physalin I ( 6), and physalin II ( 7), were isolated from the 80% EtOH extract of calyces from Physalis alkekengi var. franchetii together with 11 known steroids ( 3- 5 and 8- 15) and eight flavonoids ( 16- 23). The structures of the new compounds were elucidated primarily on the basis of 1D and 2D NMR and mass spectroscopic studies. The relative configuration of the 3-OH group of 3, 4, and 5 was also established or re-established. The inhibitory effects of compounds 1- 23 on nitric oxide production in lipopolysaccaride-activated macrophages were evaluated.     

JBIR-94 and JBIR-125, antioxidative phenolic compounds from Streptomyces sp. R56-07

Two phenolic compounds, JBIR-94 (1) and JBIR-125 (2), were isolated from the fermentation broth of strain R56-07, which was identified by phylogenetic methods as a novel species of Streptomyces. The structures of 1 and 2 were assigned on the basis of 1D and 2D NMR spectroscopy and MS analyses. Compounds 1 and 2 exhibited 1,1-diphenyl-2-picrylhydrazyl radical scavenging activity with an IC(50) value of 11.4 and 35.1 μM, respectively. These compounds are the first examples of hydroxycinnamic acid amides containing putrescine or spermidine produced by actinomycetes.     

牛膝中一个新的阿魏酰胺苷(英文)

目的:研究牛膝的化学成分。方法:采用D101型大孔吸附树脂、硅胶、ODS和制备型高效液相色谱等分离手段,运用NMR等波谱技术鉴定化合物的结构。结果:从牛膝中分离并鉴定了2个阿魏酰胺苷和7个皂苷类化合物:N-trans-feruloyl-3-methoxytyramine-4′-O-β-D-glucopyranoside(1),N-trans-feruloyl-3-methoxytyramine-4-O-β-D-glucopyranoside(2),PJS-1(3),chikusetsusaponinIVa(4),oleanolicacid3-O-[β-D-glucuronopyranoside-6-O-methylester]-28-O-β-D-glucopyranoside(5),oleanolicacid3-O-[β-D-glucuronopyranoside-6-O-ethylester]-28-O-β-D-glucopyranoside(6),oleanolicacid3-O-[β-D-glucurono-pyranoside-6-O-butylester]-28-O-β-D-glucopyranoside(7),ginsenosideR0(8)和hederagenin-28-O-β-D-glucopyranosylester(9)。结论:化合物1为新化合物,化合物2和9为首次从该植物中分离得到。     

Water-soluble ginsenosides in American ginseng]

OBJECTIVE: To have further comprehension of American Ginseng on the basis of its water-soluble components. METHOD: The water suspension of 80% methanol extract of American Ginseng was sequentially extracted with ethyl ether and n-butyl alcohol. The saccharides in the water-soluble portion were removed by macro-reticular resin column, and three compounds were obtained by silica-gel column chromatography. Their structures were confirmed on the basis of spectral analysis(IR, NMR, MALDI-MS) melting points and optical degrees. RESULT: Three compounds were identified as malonyl ginsenosides Rb1, ginsenoside Rb1 and Re respectively. Among them Rb1 and Re are known, while malonyl ginsenoside Rb1 was isolated from American Ginseng for the first time. Its structure was elucidated as (3 beta, 12 beta)-20-[(-6-O-beta-D- glucopyranosyl-beta-D-glucopyranosyl)oxy]-12-hydroxylammar-24-en-3-yl-O- [6-O-(carboxyacetyl)-beta-D-glucopyranosyl)]-beta-D-glucopyranoside. CONCLUSION: Water-soluble ginsenosides were isolated from the water-soluble extract of American Ginseng suggesting that malonyl ginsenosides exist both in American Ginseng and Ginseng.     

三七根茎的化学成分研究

目的:研究五加科人参属植物三七Panaxnotoginseng(Burk)F.H.Chen根茎中的化学成分。方法:利用大孔吸附树脂柱、硅胶柱、RP-8和RP-18柱进行化合物的分离纯化,根据其理化性质和光谱数据进行结构鉴定。结果:从三七根茎中分离得到8个化合物,分别鉴定为:人参皂苷Rh4(ginsenoside Rh4,Ⅰ),人参皂苷Rh1(ginsenosideRh1,Ⅱ),人参皂苷Re(ginsenoside Re,Ⅲ),三七皂苷R1(notoginsenoside R1,Ⅳ),人参皂苷Rd(ginsenoside Rd,Ⅴ),人参皂苷Rb1(ginsenoside Rb1,Ⅵ),三七皂苷S(notoginsenoside S,Ⅶ),三七皂苷T(notoginsenoside T,Ⅷ)。结论:化合物Ⅰ为首次从该植物中分离得到,化合物Ⅶ和Ⅷ为首次从三七根茎中分离得到。     

Cytotoxic isomalabaricane triterpenes from the marine sponge Rhabdastrella globostellata

Fourteen isomalabaricane triterpenes were isolated from the marine sponge Rhabdastrella globostellata. In addition to the known compounds globostellatic acids A (1) and D (4) and stelliferin riboside (13), 11 of the compounds were new natural products, which included globostelletin (3), eight new globostellatic acid congeners, F to M (2, 5-11), and two new stelliferin ribosides (12 and 14). The isolated compounds were tested against three different cancer cell lines, L5178Y (mouse lymphoma), HeLa (human cervix carcinoma), and PC-12 (rat pheochromocytoma). The isomalabaricane derivatives were found to be selectively active toward the mouse lymphoma cell line L5178Y. The structures were determined by 1D and 2D NMR data and by comparison with spectroscopic data of known related compounds.