冰片中右旋龙脑及其异构体的手性毛细管气相色谱法测定

以CYDEX -B手性毛细管柱 (25m×0.22mm,0.25μm)作为分析柱,用气相色谱法和气相色谱 -质谱联用法对天然冰片、艾片和合成冰片进行测定。合成冰片中的左旋龙脑与右旋龙脑可完全分离 ,左旋异龙脑与右旋异龙脑可部分分离。实验测得 :天然冰片中右旋龙脑的含量为99.13%～99.61 %;艾片中左旋龙脑的含量为95.87 %;合成冰片中左旋龙脑的含量为31.44 %～54.57 %,右旋龙脑的含量6.87 %～25.37 %;合成冰片的比旋度 α30D 为 -17.3°～ -2.3°。     

内-α-取代-α-甲基双环[2.2.1]-5-庚烯-2-基甲醇的合成及香气

许多降冰片烷衍生物可以作为食品或化妆品香精中的香原料,如珍贵的天然檀香油中的主要成份β-檀香醇(?)近年来又有许多其它作为香原料的降冰片烷衍生物的报道,例如具有如下通式的化合物     

艾纳香挥发油化学成分的气相色谱 -质谱分析

由黔产艾纳香（Blumea balsamifera DC.)的叶提取挥发油,分出结晶后的母液,用气相色谱－质谱进行定性分析和峰面积相对含量的测定,鉴定出41个化学成分;主要成分为L－龙脑、樟脑、β-石竹烯、桉叶油醇、古芸烯、芳樟醇等。     

贝母植物碱研究Ⅹ.——岷贝母中的植物碱

从甘肃岷县产的岷贝母,Fritillaria Cirrhosa Var.Roylei(HK.F.)中,提得两种新植物硷,命名为岷贝素甲及岷贝素乙。岷贝素甲为无色针状结晶,熔点210—212°,[α]_D~(12°)—73.3°(三氯甲烷),实验式测定为C_(27)H_(43)O_2N。岷贝素乙为无色菱形结晶,熔点220°,[α]_D~(16°)—52.4°(三氯甲烷),实验式测定为C_(27)H_(41)O_3N。并制得此两植物硷之硫氰酸盐,盐酸盐等。     

贡甲根中生物碱的化学研究

从芸香科植物贡甲(Acronychia oligophylebia Merr.)的根中分得了九个生物碱1～9和β-谷甾醇(10),其中吴茱萸春(1)、香草木宁(3)、原茵芋碱(4)、茵芋碱(5)和斑点弗林定(6)是已知生物碱,1,4,6三个生物碱是第一次从山油柑属植物中分得.贡甲定碱(2)和贡甲辛定碱(9)是两个新化合物.贡甲辛碱(7)和贡甲碱(8)是首次从植物中分得.用光谱方法推断了2,7,8,9的结构,由合成证明7,9的结构. 7和8具广谱抗真菌作用,但作用较弱.     

天然冰片新手性化合物的合成及其晶体结构

利用天然丰产的手性助剂冰片醇与5-羟基-2(5H)-呋喃酮反应得到液体的5-冰片氧基-2(5H)-呋喃酮差向异构体混合物,后者通过硫酚的不对称Michael加成反应,得到固体的非对映异构体混合物.进一步采用分步结晶拆分的方法,得到了光学纯新的冰片手性化合物,de>98%.通过X-射线四圆衍射确定了其立体化学绝对构型.此方法的成功为天然手性助剂的利用,为液体差向异构体混合物制备光学纯非对映体化合物提供了一条新的有效途径.     

含嘌呤、嘧啶类有机碱基的丁内酯的合成

利用天然手性助剂(-)-冰片所制得的手性源5-[(1s)-(-)-冰片氧基-2(5H)-呋喃酮差向异构体3a+3b与具有生理活性的嘌呤、嘧啶类有机碱基进行不对称Michael加成反应,得到了嘌呤、嘧啶类丁内酯非对映体混合物5a～5e及-5'a～5'e。报道了它们的合成方法以及IR、UV、^1HNMR、^1^3CNMR、MS、元素分析等结构分析数据。其中5d+5'd通过优势结晶拆分法得到单一的光学活性化合物。     

满山香中的联苯环辛二烯木脂素

满山香[Schisandra propinqua(Wall.)Hook.f.et Thoms]为五味子科植物,云南民间代五味子药用^[1],由于从五味子科植物中已分离到不少保肝降酶,抗艾滋病毒,抗癌和PAF拮抗等活性成分,其研究受到重视^[2-4],主含满山香根和提取物的复方注射液曾在云南省几所医院临床用于治疗肺癌,但其研究仅分离鉴定了两个三萜 酸([2],为进一步寻找有效成分,我们对满山香茎藤进行了研究,从中分得8种联苯环辛二烯木脂素,经波谱和分析鉴定它们的结构为：acetylgomisin R(1) angeloylgomisin R(2),gomisinA(3),gomisin B(4),gomisinN(5),gomisinO(6),6-O-benzoylgomosin O(7)和Schisantherin A(8),1为新化合物,2系首次从五味子属植物中分得,其它均为首次从满山香中分得。     

猫眼草化学成分的研究

猫眼草(Euphorbia Lunulata Bge.)是民间治疗慢性气管炎的一种草药.为阐明其有效成分,提高疗效,对猫眼草进行了化学成分的研究.利用硼砂-乙酸乙酯,聚酰胺柱层析等方法,分离到六种结晶(Ⅰ～Ⅵ).经红外光谱、紫外光谱、质谱与核磁共振谱等分析及物理化学常数的测定,鉴定出其中五种结晶(Ⅰ～Ⅴ)分别为3,5,7,4'-四羟基黄酮(山萘酚),3,5,7,3',4'-五羟基黄酮(槲皮素),山萘酚-3-单-L-鼠李糖甙,槲皮素-3-单-L-鼠李糖甙,与6,7-双羟基香豆精.Ⅵ是新化合物,其结晶经测定证明亦属香豆精类,命名为猫眼草素(Maoyancaosu).     

尼龙—1010SAXS研究

用一维电子密度相关函数方法,分析了国产尼龙-1010不同拉伸比时的SAXS现象,由实验相关函数曲线可算得长周期(L),中间层厚(d_(tr)),片晶层厚(d_?),非晶层厚(A_?),平均片层厚(d),积分不变量(Q),比内表面O_s以及(η_c-η_a)等数值及其变化规律。实验结果表明尼龙-1010的结晶结构是由结晶层、非晶层以及结晶-非品中间层三部分组成。     

新疆一枝蒿挥发油化学成份的研究

新疆一枝蒿挥发油有明显的抗过敏作用。通过 GC/MS/DS 分析,表明有三十九种化学成份,并确证了其中十八种的结构及含量。     

千山野菊花挥发性化学成分的提取与分析

报道了用蒸馏-萃取法和同时蒸馏-萃取法提取千山野菊花中挥发性物质，测得用两种方法提取的千山野菊花挥发油含量分别为6．1％和7．0％，用GC／MS法从千山野菊花挥发油中分别分离并确定出34种和29种化学成分，分别占千山野菊花挥发油总检出量的89．47％和90．72％，用峰面积归一化法得出各类化学成分在挥发油中的相对百分含量。     

COMPOSITION OF THE ESSENTIAL OIL OF Arbutus unedo

Water-distilled essential oil from leaves ofArbutus unedoL. of Turkish origin was analyzed by GC/MS. Thirty-seven constituents were characterized with (E)-2-decenal (12.0 %), -terpineol (8.8 %), hexadecanoic acid (5.1 %), and (E)-2-undecenal ( 4.8 %) as the major constituents.     

GC／MS法测定木香挥发油化学成分

用气相色谱-质谱法对木香挥发油进行化学成分的分析。采用水蒸气馏法从木香中提取挥发油。试用不同类型的毛细管柱进行分析,找出最佳分析条件,用归一化法测定其含量,并用气相色谱-质谱法对化学成分进行鉴定。共鉴定了38个成分,占挥发油总成分的86%以上。方法稳定可靠。重现性好,适用于中药挥发油的化学成分分析。     

气相色谱-质谱法分析木奶果挥发油的化学成分

采用水蒸汽蒸馏法从大戟科木奶果中提取挥发油,用气相色谱-质谱对挥发油的化学成分进行了分析。鉴定出19种化合物,占总油量的100%,用面积归一化法测定了各成分的相对百分含量。木奶果挥发油主要成分为正十六碳酸、丁基甲氧基苯、9,12-十八碳二烯酸,分别占挥发油总量的29.53%、17.47%和11.59%,三者占其总量的58.59%。     

啤酒无机成分分析进展

综述了国内外啤酒无机分析的情况,侧重介绍了等离子体发射光谱(ICP-AES)技术的应用研究.     

COMPOSITION OF THE ESSENTIAL OIL OF Haplophyllum myrtifolium

The chemical composition of the essential oil ofHaplophyllum myrtifoliumBoiss., endemic to Turkey, was examined by GC/MS. Ninety-seven compounds were characterized with linalool (12.8%), -caryophyllene (10.3 %), and methyleugenol (5.9 %) as the main constituents.     

抗肿瘤多酸药物[Mo7O24]6-的电子结构研究

运用第一原理密度泛涵理论中的离散变分方法（ＤＦＴ－ＤＶＭ）对具有抗肿瘤活性的多酸药物三合水七钼酸异丙基胺的阴离子「Ｍｏ７Ｏ２４」＾６－进行了电子结构，获得了键级、不等价原子的电子占据数、原子净电荷，分子轨道能级以及「Ｍｏ７Ｏ２４」＾６－的ＨＯＭＯ和ＬＵＭＯ组成等数据，并对该药物的活性和作用机理从电子结构的角度进行了讨论。     

Studies on chemical constituents of Flos Puerariae-Semen Hoveniae medicine pair by HPLC and Fourier transform ion cyclotron resonance mass spectrometry

Alcoholic liver disease is currently the most clinically concerning liver disease, which occurs from chronic alcohol abuse. Flos Puerariae and Semen Hoveniae have been used to treat alcohol drinking excessively for thousands of years in China. In this study, the ethanol extract of the medicine pair was qualitatively and quantitatively analyzed by high-performance liquid chromatography and Fourier transform ion cyclotron resonance mass spectrometry. First, the high-performance liquid chromatography fingerprint was established to obtain the overall chromatographic data of its chemical constituents. Next, high-performance liquid chromatography-mass spectrometry was applied to identify its chemical constituents. Then, the characteristic constituents were simultaneously quantified by high-performance liquid chromatography. In addition, the chemical constituents that were absorbed into rat plasma were identified by high-performance liquid chromatography-mass spectrometry. As a result, a total of 48 chemical constituents in the medicine pair were detected and identified in vitro. Meanwhile, the content of seven representative constituents, including dihydromyricetin, glycitin, genistin, tectoridin, glycitein, genistein, and tectorigenin were simultaneously determined. Furthermore, a total of 19 chemical constituents were detected in rat plasma after oral administration. In short, the chemical constituents of the medicine pair were initially investigated in this study, which will lay the foundation for the discovery of its pharmacodynamic substances in further works.     

Variability of volatile constituents in Artemisia maritima in western Himalaya

Chemical composition of the essential oil of Artemisia maritima, collected from three different high altitude locations in western Himalaya was studied by gas-chromatography mass spectrometry. Twenty-five constituents were identified in the oil distilled from the sample from Pooh, of which 1,8-cineole (23.8%) and chrysanthenone (17.54%) were the major constituents. Twenty volatile constituents were identified from the sample collected from Rhongtong pass, of which chrysanthenone (38.1%) and 1,8-cineole (37.3%) were the major constituents. In the oil distilled from the sample collected from Lahaul-Spiti 28 constituents were identified, of which 1,8-cineole (44.22%), camphor (9.16%) and borneol (10.94%) were the major constituents. In this sample chrysanthenone was present in very low percentage.