高效毛细管电泳的电导检测和紫外光度检测研究

本文自制商效毛细管电泳装置.研究了毛细管区带电泳电导检测和毛细管胶束电动色谱紫外光度检测。在电导检测中,制作铂丝微电导池,并由用电池隔膜制作的导电接口连接电泳毛细管和电导池,高压被有效隔离,实现柱后电导检测,用内径200μm、长70cm(到接口)石英毛细管在10kV电压下分离检测Li~-、Na~-、K~-。在电动色谱中将高效液相色谱仪与高压电源组成电泳装置,用内径100μm,长50cm(到检测器)石英毛细管和SDS胶束溶液在14kV电压下分离检测电中性化合物。     

一种简易型毛细管电泳电导检测装置及其应用

报道了一种简便、实用的毛细管电泳电导检测装置 ,该装置使用毛细管微铂丝为敏感电极 ,大面积铂电极为参比电极 ,并以一根不锈钢针管为连接导管 ,成功地实现了毛细管电泳的柱端式电导检测 ,并对K 、Na 、Li 3种碱金属离子进行了分离检测。实践表明 ,该装置具有制作简单且成功率高、更换电极方便的特点。在所选的实验条件下 ,3种金属离子在1×10 -5～1×10 -3mol/L浓度范围内电泳峰与浓度呈良好线性关系 ,检出限为5×10-6 mol/L。应用该法对城市自来水样品进行了测定 ,其重现性和检测结果令人满意     

毛细管电泳高频电导法同时测定阿莫西林和克拉维酸钾含量

毛细管电泳高频电导法同时测定阿莫西林和克拉维酸钾含量;毛细管电泳; 高频电导检测; 非接触式电导检测; 阿莫西林; 克拉维酸     

毛细管电泳多道电化学检测器的研制及其应用

报道了毛细管电泳多道电化学检测器的研制及其应用，安培检测器和电导检测器并联在同一毛细管电泳检测系统中，在同一缓冲体系，同一工作电极下对同一复杂的分析体系同时进行电导和安培检测；整个装置综合了电导检测和安培检测两种检测器的优点，性能优良，造价低廉，对实际样品的检测取得了令人满意的结果。     

毛细管电泳安培及电导检测最新进展

对毛细管电泳安培检测和电导检测的研究近况进行了综述,分别介绍了电导法和安培法与毛细管电泳的联接及应用,并对其发展方向作了展望。     

新型微型电导池的研制及共地效应的消除

使用简便的方法制作了电极面积大、无死体积、分辨率高、检测限低的微型电导池;较好地消除了毛细管电泳(CE)在柱电导检测装置中存在的共地效应,排除了在线检测时高压分离回路对电导检测回路的干扰.并对制作的微型电导池的性能进行了测试.     

稀土离子及胺和氨基酸的高效毛细管区带电泳电导检测

用自制高效毛细管电泳装置研究毛细管电泳电导检测，由用阴离子交换膜管制作的导电接口连接电泳毛细管和电导池，高电压被有效隔离，实现柱后电导检测，用长６０ｃｍ、内径５０μｍ石英毛细管，以ｐＨ４．０的７×１０￣（－３）ｍｏｌ／ＬＮａＡｃ￣（－２）×１０￣（－３）ｍｏｌ／ＬＨＩＢＡ－ＨＡＣ溶液为载体，在１８ｋＶ电压下，轻重三种稀土Ｎｄ、Ｇｄ、Ｙｂ的混合物８ｍｉｎ内完成分离检测。用上述毛细管，以ｐＨ为５．８的５×１０￣（－３）ｍｏｌ／ＬＮａＡｃ－ＨＡＣ溶液为载体，在２０ｋＶ电压下乙二胺、三乙胺、组氨酸、谷氨酸混合有机物７．５ｍｉｎ内完成分离检测。     

毛细管电泳与芯片毛细管电泳的双检测技术

综述了毛细管电泳和芯片毛细管电泳的3种双检测技术,包括荧光-散射等光学双检测技术、安培-非接触电导等电化学双检测技术和荧光-非接触电导等光电联用双检测技术.介绍了3种双检测方法的仪器的检测原理及应用,并展望了双检测技术的发展前景.引用文献54篇.     

体液中卡托普利的乙醚提取毛细管电泳法测定

体液中卡托普利的乙醚提取毛细管电泳法测定;毛细管电泳;高频电导检测;非接触式电导检测;卡托普利;体液     

新型微型电导池的研制及其地效应的消除

使用简便的方法制作了电极面积大、无死体积、分辨率高、检测限低的微型电导池;较好地消除了毛细管电泳ＣＥ）在柱 存在的共地效应,排除了在线检测时高压分离回路对电导检测回路的干扰。并对制作的躲开电导池的性能进行了测试。     

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.