FAAS法分析当归、黄芪及当归补血汤中金属元素的形态

采用正辛醇-水分配体系模拟中药水煎液在人体肠胃中的分配情况,应用火焰原子吸收光谱法测定了当归、黄芪及当归补血汤中锌、铁、锰、铜、镁、钙、镍7种金属元素在药材中的总含量,以及水煎液中各金属元素的水溶态、醇溶态含量,探讨了配伍和酸度对水煎液中金属元素含量的影响。实验结果表明,中药中金属元素的形态与中药成分、配伍情况及作用靶位(肠胃)的酸度有关,配伍及酸度对中药中金属元素的溶出率及水煎液中金属元素的形态影响较大。     

广西黑老虎中微量元素测定

采用原子吸收光谱法测定广西黑老虎中锰、铁、铜、锌、镁、钙等6种微量元素，并与笋干和16种蔬菜中6种微量元素含量进行比较，结果发现，黑老虎中锰、铁、铜、锌、镁、钙等6种微量元素含量均较高，其中锰、钙、铜、锌含量高于笋干，锰、铁、铜、锌含量远远高于16种蔬菜中微量元素的含量，钙含量高于部分蔬菜含量。提示广西黑老虎中含有丰富的人体所需微量元素，作为药用植物，具有极高的药用价值。     

火焰原子吸收光谱法测定复方丹参片中微量元素各形态含量

采用火焰原子吸收光谱法对复方丹参片水煎液及人工胃酸提取液中具有生物活性的微量元素铁、铜、锰和锌的形态分布进行了研究。用OasisTMHLB固相提取小柱分离药物的两种提取液中所述4种元素的无机态和有机态;用D401螯合树脂分离4种元素的稳定态和不稳定态;用Amberlite XAD-7大孔吸附树脂分离得到与丹酚酸的有机结合态。结果表明:锌、铜的蛋白质结合态分布较高,多糖结合态中以铜元素为主,丹酚酸有机结合态中铁元素的含量最高。     

中草药龙胆中微量元素的形态分析

采用传统煎煮法对丽水当地中草药龙胆中钙、锌、铁、铜、锰、铅、镉和铬等8种元素进行提取,并用微孔滤膜分离提取液中可溶态与悬浮态;利用大孔吸附树脂分离可溶态中有机态与无机态;采用正辛醇/水分配体系模拟水煎液中这8种微量元素在人体胃肠中分配情况,再用火焰原子吸收光谱法(FAAS)测定了各种形态中的8种元素。研究结果显示:龙胆中8种元素的提取率在34.25%～74.53%,浸留比在49.58%～371.1%,悬浮态颗粒吸附率在6.5%～29.8%,该法对各元素的加标回收率在91.3%～108.5%;相对标准偏差小于3.5%;锌、铁、铜、锰在正辛醇/水分配体系中溶出性受酸碱性影响大些。     

全蝎中4种微量元素的形态分析

对中药全蝎中铜、锌、铁和镁4种微量元素存在的形态及含量进行了研究。文中叙述了全蝎样品中元素的各种形态(可溶态、悬浮态、无机态、有机态)的提取方法和分离,采用火焰原子吸收光谱法测定了各试液中4种微量元素的含量。结果显示,全蝎中4种元素的总提取率在39.9%~63.2%之间,浸留比在73.6%~126.0%之间,悬浮态颗粒吸附率在10%左右,铜、锌、铁、镁的有机态与无机态的比例在250.0%~550.0%之间。     

七种香烟中锌,铜,铁,锰,镍含量的分析

用原子吸收法测定了７种香烟的５种微量元素的含量，结果表明，７种香烟中锌，铜，锌，锰，镍的含量存在的较大差异，其中以铁，锰含量较丰富，镍含量较少，本测定为探讨香烟中的微量元素与疾病的关系提供了有用数据。     

糖尿病母亲及其新生儿全血14种微量元素的研究

为了解糖尿病母亲及其新生儿全血微量元素的分布情况，采用日本岛津ICPQ－1012型高频等离子体发射光谱仪检测了糖尿病母亲及其新生儿的全血14种微量元素。以正常产妇及足月新生儿病例为对照组，观察糖尿病母亲及其新生儿的全血14种微量元素的改变。结果糖尿病母亲铜元素高于正常产妇，铬、锰、锌元素低于正常产妇，糖尿病母亲新生儿铜元素高于正常新生儿，锌、锰、镁、铬元素低于正常新生儿。糖尿病母亲新生儿镁、镍、铜、锌、钙、钼、锶、铁低于糖尿病母亲。结论：糖尿病母亲血铬、锌、锰元素低于正常，铜元素增高是由于糖尿病疾病所引起，糖尿病母亲新生儿铜元素增高，血镁、钙、锰、锌等低于正常，与糖尿病母亲本身微量元素特点有关。糖尿病母亲新生儿血镁、镍、铜、锌、钙、钼、锶、铁元素低于糖尿病母亲与先天发育不足有关。     

六种生物制剂中锌、铜、铁、铬、锰、镍含量的测定

利用火焰原子吸收法直接测定生物制剂样品中锌,铜,铁,铬,锰,镍的含量。结果表明,六种生物制剂中以蚂蚁因子注射液中的铜、铜,铁,铬,锰,镍含量最高;不同的生物制剂中六种微量元素的含量有一定差别。     

杜仲叶水煎及醇提液中无机元素赋存形态分析

通过水煎及醇提法对杜仲叶中铁、锌、铜、锰、钾、钠、钙和镁8种无机元素进行提取,分别用微孔滤膜、D101大孔树脂、732阳离子树脂、D402螯合树脂将无机元素分为初级形态及次级形态。采用环己烷-正丁醇分配体系模拟人体肠胃条件将无机元素分为脂溶态和水溶态,用火焰原子吸收光谱法(FAAS)对各种形态的无机元素进行测定。结果表明:杜仲叶醇提液中各无机元素提取率均高于水煎液;杜仲叶醇提液中8种无机元素的提取率为6.61%~89.30%;次级形态分析参数表明各无机元素均以某种次级形态为主的多种形态共存于可溶态溶液中。该法测定各元素的回收率为98.99%~104.0%,相对标准偏差在0.35%~1.11%之间,具有良好的精密度和准确度。     

火焰原子吸收光谱法测定抗癌中草药中11种微量元素

采用在600℃灰化法处理样品,浓硝酸溶解灰化残渣,溶液定容为50 mL,用火焰原子吸收光谱法测定了20种抗癌中草药中钙、锾、锰、铜、铁、锌、镉、铅、钴、镍、铬等11种微量元素.结果表明:抗癌中草药中除含有丰富的钙、镁、铁外,还含有较高含量的锌、锰、铜等对人体有益的微量元素.以丹皮样品为基体,加入11种元素的标准溶液作回收试验,回收率在92.3%～107.5%之间,相对标准偏差(n=5)在2.1%～5.2%之间.     

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.