顶空气相色谱-质谱法分析补骨脂挥发油化学成分

采用顶空气相色谱-质谱(Headspace/GC-MS)联用技术对补骨脂挥发油化学成分进行分析,确认出65种组分,并用峰面积归一化法测定,其质量分数占总挥发性组分峰面积的93.30%。主要成分为:乙酸乙酯(1.61%)、芳樟醇(3.56%)、反-石竹烯(26.8%)、白菖油烯(4.48%)、α-律草烯(3.28%)、1s,顺-卡拉烯(3.16%)、石竹烯氧化物(9.83%)和异补骨脂素(3.02%)。     

顶空固相微萃取GC-MS分析紫云英蜂蜜的香味成分

建立了顶空固相微萃取-气相色谱-质谱联用(HS-SPME-GC-MS)分析紫云英蜂蜜香味成分的方法。采用质谱谱库检索结合化合物保留指数定性分析色谱峰,面积归一化法进行定量分析。从紫云英蜂蜜中分离了68个组份,定性了其中的49个,占总峰面积的92.24%。紫云英蜂蜜香味的主要成分为醛类(61.2%)、醇类(14.29%)和酯类(2.38%)。     

GC-MS分析大蒜中的挥发油和大蒜精油

采用气相色谱—质谱法，分析比较大蒜中的挥发油以及大蒜精油的化学成分，通过非负矩阵因子分解(NMF)方法解析色谱重叠峰，并用峰面积百分比法计算各化学成分的峰面积相对百分含量。确定了大蒜中37种化学成分，其中含硫化合物34种，大蒜精油中的32种化学成分，含硫化合物28种。     

气相色谱-质谱法测定废旧印刷线路板真空热解油的组分

采用气相色谱-质谱法从废旧印刷线路板的真空热解油中分离并确认出21种化合物,与红外光谱分析所推断的结果相一致,并用峰面积归一化法得出各化合物的相对含量.结果表明:热解油组分经过DB-5非极性柱可以实现分离,油中相对含量较高的主要成分为苯酚(30.17%)、对异丙基苯酚(10.29%)、对苯基苯酚(13.93%)、对异丙烯基苯酚(8.21%)和双酚A(15.46%).     

气相色谱-质谱联用分析茶树油的成分

采用常规水蒸气蒸馏法从茶树枝叶中提取茶树油，经气相色谱-质谱联用分析，分离出47种成分，检索NI蚋8质谱数据库，与标准谱图对照鉴定了其中32种成分。应用Hewlett—Packard软件，按峰面积归一化法定量，所鉴定成分的馏出峰面积占总馏出峰面积的96．08％。     

鸢尾根挥发性成分的GC-MS分析

采用气相色谱-质谱联用技术对罗布麻的挥发性成分进行了分离鉴定。分离出40种成分,共确认了其中26种成分,占挥发油总含量的86.6%。采用峰面积归一化法确定了各成分的相对含量,其中主要成分为3-甲氧基-1,2-丙二醇(29.54%)、月桂酸(12.04%),癸酸(4.52%)、9,12-十八碳二烯酸甲酯(4.15%)、棕榈酸(3.91%)、月桂酸乙酯(3.87%)、庚烷(3.74%)、肉豆蔻酸(3.69%)。     

基于组效关系的姜黄挥发油抗肿瘤活性成分辨识研究

基于GC-MS分析,建立了姜黄挥发油的化学成分与其抑制人宫颈癌Hela细胞作用的组效关系模型,寻找与药效显著相关的活性成分。采用水蒸汽蒸馏法提取得到31批姜黄挥发油,提取率在1.63%～4.52%之间;采用GC-MS联用仪建立了31批姜黄挥发油的指纹图谱,确定了20个特征峰,以特征峰的相对峰面积(各峰面积与内标正十三烷的峰面积之比)来表征其相对含量;MTT法测定姜黄挥发油抑制人宫颈癌Hela细胞活性,以抑制率为评价指标;利用Simca-p11.5软件的正交投影偏最小二乘法(Orthogonal Partial leastsquares,OPLS)和SPSS软件的双变量相关(bivariate)分析,研究特征峰与药效的相关性,根据S-载荷图、变异权重参数值(Variable importance in projection,VIP)和皮尔逊(Pearson)相关系数来辨识显著活性成分。结果表明,11,15,7,19,3,6,12,14,9号等9个特征峰与姜黄挥发油抑制Hela细胞活性显著相关,除19号峰尚未定性外,11,15,7,3,6,12,14和9号峰对应的成分分别为芳姜黄酮、β-姜黄酮、姜烯、β-榄香烯、α-姜黄烯、α-姜黄酮、吉马酮和β-倍半水芹烯。     

鸢尾根挥发性成分的GC-MS分析

采用气相色谱-质谱联用技术对罗布麻的挥发性成分进行了分离鉴定.分离出40种成分,共确认了其中26种成分,占挥发油总含量的86.6%.采用峰面积归一化法确定了各成分的相对含量,其中主要成分为3-甲氧基-1,2-丙二醇(29.54%)、月桂酸(12.04%),癸酸(4.52%)、9,12-十八碳二烯酸甲酯(4.15%)、棕榈酸(3.91%)、月桂酸乙酯(3.87%)、庚烷(3.74%)、肉豆蔻酸(3.69%).     

气相色谱-质谱联用分析白兰叶油成分

采用气相色谱－质谱联用技术对苏州产白兰叶油的化学成分进行了分析,分离出３３个峰。鉴定了其中２７种成分,占总峰面积的９７％,并对油中的主要化学成分芳樟醇用气相色谱－傅立叶红外光谱法进行了验证。     

糖胶树叶挥发油化学成分研究

采用水蒸气蒸馏法提取糖胶树叶的挥发油.运用气质谱联用(GC-MS)技术研究海南糖胶树叶的挥发油化学成分.并采用峰面积归一化法确定各成分的相对质量分数.结果共鉴定出36种成分,占总离子流出峰面积的94.83%.糖胶树叶挥发油主要有α-蒎烯(16.62%),2-丙烯酸丁酯(15.86%)和大根香叶烯D(13.37%).本研究可为糖胶树的进一步研究开发和利用提供基础研究数据.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.