Perfluoroalkyoxy-substituted cyclohexene oxides(EFPO1 and EFPO2) were obtained by two-step reactions using the dimer and trimer of hexafluoropropylene oxide and 4-cyclohexene-1,2-dimethanol as main raw materials.The structures of as-synthesized products were confirmed by spectroscopy analyses including FT-IR and 1H NMR.These fluoro-epoxides are compatible with the prepolymers such as bisphenol-A diglycidyl ether and ethylene glycol diglycidyl ether,thereby endowing the coatings composed of them with improved hydrophobicity as evidenced by the photoinitiated curing experiments.The preliminary investigation of their UV-curing performance shows that the hydrophobicity increases linearly with increasing fluoro-epoxide content in the composition.As expected,the hydrophobic effect is more pronounced for EFPO2 than EFPO1 at the same conditions,because the former has a longer ferfluoroalkyoxy group.For example,upon addiing 1% mass fraction of EFPO2,the water contact angle of the UV-cured films was 99° and was higher 14° than that found for the films without the fluoro-component,whereas the value for EFPO1-modified films was 87°.When containing 5% EFPO2,high hydrophobic surface was achieved with a water contact angle of 113 for the UV-cured films.In addition,it should be pointed out that the hydrophobic surface can be further improved by heating the UV-cured films at 110 ℃ for 6 h.For the coatings containing 1%~5% EFPO2,the post-heating treatment resulted in a change of the water contact angles from the range 99°~113° to 113°~118°,while the changes were from 87°~100° to 99°~110° for EFPO1 analogs.The thermal migration of fluoro-chains and aggregation on the film surface seems to be responsible for the enhancement in hydrophobicity.Consequently,this new type of fluorine-containing epoxy monomers is expected as the surface modifier used in coatings,inks and release materials.

A method for separation and determination of spin-labeled anti-tumor podophyllotox in derivatives by HPLC coupled with electron paramagnetic resonance(EPR) has been developed.The analytical conditions of reverse phase HPLC have been discussed and an separation of GP-3,GP-5,GP-7 was obtained by using MeOH-H2O system.The detection limits were 10-8g/mL.EPR detector was then used to determine HPLC.This new technique has been proved to be useful for pharmacokinetics study of spin-labeled anti-tumor podophyllotoxin derivatives.This method was assayed.It is simple,rapid and accurate.

OBJECTIVE:To study the polysaccharide of Condonopsis pilosula.METHOD:The polysaccharide, CPP-1, was purified by DE-52 cellulose and Sephadex G-200 gel column chromatography. Purity and molecular weight of the polysaccharide were determined by gel permeation chromatography. Methylation analysis, periodate oxidation and degradation, IR, 1H-NMR and 13C-NMR methods were adopted to elucidate the chemical structure.RESULT:The molecular weight of CPP-1 was estimated to be 7.5 x 10(4), and the structure of CPP-1 was a beta-(2 --> 1) linked beta-D-fructosan.CONCLUSION:CPP-1 was a neutral homosaccharide.

Five compounds, terephthalic acid mono-[2-(4-carboxy-phenoxycarbonyl)-vinyl] ester (1), (E)-3-(5′-hydroperoxy-2,2′-dihydroxy[1,1′-biphenyl]-4-yl)-2-propenoic acid (2), 3,4,5-trihydroxybenzoic acid (3), succinic acid (or butanedioic acid) (4), and 2,3,4,5,6-pentahydroxybenzoic acid (5), were isolated from Phyllanthus urinaria . The structures of these compounds were elucidated by means of spectral techniques including IR, MS, and 1D/2D NMR. 1 and 2 are new compounds.

α-D-Glucan (ASP-1) was isolated from the hot water extract of Angelica sinensis roots by ethanol precipitation, anion-exchange and gel-permeation chromatography. Smith degradation, NMR spectroscopy, composition and methylation analyses confirmed the ASP-1 structure comprises a (1→6) linked α-D-glucopyranosyl backbone, coupled with two branches per unit bonded through α(1→3) linkages, where each branch contains Glc-(1→3)-Glc-(1-and Glc-(1→4)-Glc-(1- chains at either end.

Two novel ent-kauranoids with new sub-skeleton types, gesneroidins G and H were isolated as white powder from the ether extract of the leaves of Isodon gesneroides through normal phase column chromatography. Their structures were elucidated as 3beta,6alpha,7beta-triacetoxyl-15-hydroxyl-14-oxo-ent-15,16-seco-kaur-11,17-olide and 1alpha-hydroxyl-3beta,6alpha,7beta,11beta-tetraacetoxylent-nor-15,17-kaur-8,16-olide on the basis of the spectral evidences including ID and 2D NMR spectra.

Friedelin was first isolated from Phyllanthus niruri linn. Its structure was determined by means of spectroscopy methods and X-ray crystallography. Chemical shifts of all carbons and protons were assigned based on the 2D NMR methods. The structure elucidated by means of NMR coincided with the structure got from X-ray diffraction method. It means that structure of friedelin in crystal an in solution have a same configuration. This compound crystallized in the orthorhombic space group P2(1)2(1)2(1) with a = 6.361(2)A, b = 13.933(3)A, c = 28.440 (6)A, α = 90°,β= 90°, γ= 90°,V = 2520.6(11)A3,Z= 4.A slightlyintermolecular contact C-H O=C was observed firstly in this crystal. This contact was supposed to be the determinative factor of formation of the crystal.

毛莨科翠雀属(Delphinium)植物主要分布在北温带,我国约有近120种翠雀属植物[1],广泛分布在西藏、四川西部、青海和甘肃,生于海拔2100～4000米山地草坡或多石砾山坡,其中许多是著名的中药,具有镇痛、消炎、抗菌治疗心血管病、抗癌等功效[2],陈耀祖院士等曾对川西翠雀和甘肃南部的蓝翠雀中二萜生物碱的提取分离及结构鉴定进行了研究[3],考虑到同一种植物生长的环境不同,所含化学成份也不尽相同,我们选择了青海翠雀进行了研究[4],以充分利用和开发我国的药用植物资源.中药的神奇功效体现在多种成分的协调作用,对中草药进行多个部位,多种成分的综合研究是中药现代研究的发展方向[5],本文用GC-MS对青海翠雀花挥发油的化学成分进行了研究.

The chemical constituents have been isolated from Delphinium tatsienense Franch Var Chinghaiense by column chromatography and preparative thin layer chromatography. The structures of the diterpenoid alkaloids were elucidated by IR, EA, MS, H-1 NMR, C-13 NMR as well as DEPT. Six compounds were obtained, among which one is a new ditepenoid alkaloid, four axe known diterpenoid alkaloids and the other is P-sitosterol.

A new screening approach for anticancer active compounds is presented. In this method, a target enzyme is incubated with a mixture of compounds, and then the complex formed by the target and small molecules is separated from the rest of the mixture by ultra-filtration. The complex that is retained on the membrane is subsequently washed with acid and small molecules that are specifically bound to the target are released and collected, then analyzed by highperformance liquid Chromatograph combined with electrospray ionization mass spectrometry (HPLC/ESI-MS) analysis. We have successfully applied this method to screen anticancer compounds. DNA topoisomerase II is used as a target to capture anti-tumor candidates from a mixture of combinatorial compounds, such as doxorubicin, daunorubicin and pravastain.

建立了一种生物亲合超滤新方法, 以解决抗癌活性物质的快速筛选问题. 生物亲合超滤法的设计是以拓扑异构酶Ⅱ(TOPOⅡ)作为靶酶, 对蒽环类的拓扑异构酶抑制剂阿霉素和柔红霉素进行筛选, 并以调血脂药物普伐他汀作为对照, 结合高效液相色谱和质谱技术对筛选出的物质进行快速分析, 取得了较好的结果.

The title compound was obtained as a by-product in a contraction reaction by using DIC as a coupling reagent. X-ray diffraction shows the title compound is a pyrrolinenitroxide radical urea. Two crystallographically. Independent molecules possess different conformations but the identical bond distances and angles. Based on the molecular structure a possible reaction mechanism is proposed for the reaction of DIC and carboxylic acid.

Objective: To develop a method for the determination of ligustilide in Angelica sinensis essential oil. Methods: GC - MS method using American HP 5973 GC - MS apparatus, HP - 5 (30 m ×0. 25 mm × 0. 25 μm) capillary column, HP chemical station, NIST MS library and HP7683 autosampler. The carrie gas is heli-um. Column temperature rises by programming. The injector temperature is 250℃ and the detector temperature is 280℃. Ligustilide was determined by means of GC - MS with selected ion and qualifier ion monitoring. Results: The Standard curve is linear for ligustilide within 1. 34 ng -1. 34 pg and the sensitivity is 0. 1 ng · mL-1 ( S/N = 10). The average recovery is 98. 9% and RSD is 2. 2% . Conclusion: The results show this method is sensitive, rapid and accurate.

A new guaianolide, notoserolide E, along with nine known compounds was isolated from the Chinese endemic plant of Notoseris henryi ( Dunn) Shih and its structure was elucidated by means of spectroscopic evidence.

Fourteen compounds including eight triterpenoids, 12-oleanaen-3beta-ol (beta-amyrin) (1), 12-oleanaen-3beta-caffeate (2), 9(11),12-oleanadien-3beta-ol (3), 9(11),12-oleanadien-3-one (4), 9(11),12-oleanadien-3beta-caffeate (5), friedela-3-one (friedelin) (6), friedela-3-one-29-ol (7), and 12-gammateraen-3beta-ol (tetrehymanol) (8); one steroid, beta-sitosterol (9); one long-chain acid, octadecadienoic acid (10); two esters, ester of n-octaolecyl-4-hydroxy-cinnamate (11), and ester of n-octadecyl-caffeic acid (12); one diterpene, 8beta,19-dihydroxy-3-oxopimar- 15-ene (13); one sesquiterpene, 1beta,2beta,9alpha-trihydroxy-beta-dihydroagarofuran (14) were isolated from the aerial part of Celastrus hypoleucus, These compounds were characterized and identified by physical and spectral methods. All compounds were isolated for the first time from this plant. Among them 12-oleanaen-3beta- caffeate (2) and 9(11),12-oleanadien-3beta-caffeate (5) are two new compounds, and ester of n-octadecyl-caffeic acid (12) possessed antilipoperoxidative effect by specifically scavenging the hydroxyl free radical (.OH) in vitro.

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The structures of three new compounds isolated, from the whole plants of Oxyria digyna (L.) Hill have been elucidated to be oxyriaflavonol (1), 5, 7, 3'-trihydroxy-4-methoxyflavanone-7-O-(2"-O-beta -D-glucopyranosyl)-alpha -L-rhamnopyranoside (2) and 5, 7, 2', 3', 4'-pentahydroxyflavone-8-C-glucopyranoside (3) on the basis of spectral data. Five known compounds isolated have been identified as vitexin (4), orientin (5), hesperedin (6), quercetin-3-O-beta -D-glucopyranoside (7) and stigmasterol (8).

AIM To investigate the chemical constituents from the whole plant of the endemic plant Notoseris rhombiformis Shih. METHODS Column chromatography was used for separation and purification, while spectral analysis was used for structure elucidation. RESULTS Eight compounds were isolated from the whole plant of this Chinese endemic plant and their structures were elucidated as notoserolide A (1), notoserolide D (2), austricin (3), jacquilenin (4), 3 beta, 14-dihydroxy-11 beta, 13-dihydrocostunolide (5), p-hydroxyphenylacetic acid (6), luteolin-7-O-beta-D-glucopyranoside (7) and daucosterol (8), respectively. CONCLUSION All compounds were isolated from this plant for the first time. Among them, 2 is a new compound.

鬼臼经乙醚脱脂后用热水抽提,用蛋白酶法和Sevag法相结合除去蛋白质,乙醇分级沉淀,经DEAE-Sepharose和Superdex G-75或Sephacryl S-200HR柱层析纯化得到两种多糖组分EPS-A和EPS-B.经分析该两种多糖均为单一组分.用分子筛层析法测定EPS-A和EPS-B的分子量分别为15 kD和175kD.纸层析和气相层析分析得知,EPS-B含有木糖、阿拉伯糖、鼠李糖、葡萄糖、甘露糖和半乳糖,其摩尔比为0.37:2.20:0.57:9.83:1.0:3.42,而EPS-A中仅含葡萄糖.体内试验结果表明,EPS-B多糖对小鼠腹水肝癌细胞生长有一定的抑制作用.