毛细管电泳柱上安培检测装置的研制

介绍了一种新的毛细管电泳柱上安培检测装置。以碳纤维微电极为工作电极,在自组装的ACS－2000毛细管电泳仪上,测定了三种苯二酚的异构体：邻苯二酚、对苯二酚、间苯二酚,在20min内达到了基线分离。     

高效毛细管电泳安培检测器的研制

介绍了一种结构简单的毛细管电泳安培检测器。该检测器通过一只内径与毛细管外径相仿的不锈钢针头作分离毛细管与毛细管工作电极的导引管解决了工作电极与分离毛细管的对接 毛细管碳糊电极为工作电极,在内径为５０μｍ毛线管邮几种酚类化合物,结果表明该系统性能优良。     

高效毛细管电泳的离柱安培法检测

设计了一种新型的毛细管电泳离柱安培法检测装置,无需截断毛细管,直接使用氢氟酸蚀刻毛细管管壁制作导电接口,可有效地耦合毛细管电泳分离和安培法检测,隔离高压电场对安培法检测的干扰,实现多组分的高效分离和检测。所设计的系统性能优良,导电接口制作简便,耐用性好,无附加体积。     

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     

毛细管电泳装置及其制造方法

本发明揭示一种毛细管电泳装置以及一种制造该装置的方法。该毛细管电泳装置包括一个装置主体结构，其具有复数个排列在其上以填充样本的储存槽，以及复数列横向地定义用来与该等储存槽连接的凹沟，该等凹沟用以放置至少一个毛细管电泳芯片。该毛细管电泳芯片包括一条直线型主要分离信道、一条注射信道以及复数个定义在其上以与该等储存槽进行液体流通的样本传输通道。     

毛细管电泳流动注射-负压进样装置的研究

设计了一种用于毛细管电泳系统的流动注射-负压进样装置。样品由蠕动泵输送到进样阀后再由缓冲液带到分离毛细管入口,由毛细管出口端施加的负压引入。进样时间由自制精密控时电路控制,经进样条件的优化,能获得良好的重现性。实验中两种阳离子峰面积和迁移时间的RSD(n=8)≤2.7%,优于传统重力进样,而且操作简便;与非接触电导检测器组装成流动注射-毛细管电泳系统,可实现快速、高效的在线分析。初步应用于无机阳离子的分离,取得了满意的结果。     

基于复合型微流控芯片的紫外检测毛细管电泳系统

提出了一种基于芯片-毛细管复合装置的紫外检测-微流控芯片毛细管电泳分析系统.采用小死体积的耦合技术实现了石英毛细管与“十”字通道型微流控玻璃芯片的耦合.本系统的紫外检测灵敏度与商品化毛细管电泳仪相当.采用夹流进样方式,达到较高的进样重现性,2mmol/L苯甲酸的峰高相对标准偏差(RSD)为1.5%(n=11).可用于复方磺胺甲唑片剂的两种有效成分的快速分离.     

毛细管电泳氢化物发生等离子体原子发射光谱联用的接口设计

设计了一种毛细管电泳氢化物发生装置。应用该装置将毛细管电泳(CE)分离后的两种硒形态转化为氢化物,然后再将氢化物引入到电感耦合等离子体原子发射光谱(ICP-AES)中进行检测。讨论了盐酸、硼氢化钠的浓度和载气流速对硒氢化物发生的影响,通过两根PTFE管并列方式消除了体系的反压,将优化的条件应用于Se的形态分析,RSD小于5%,检出限低于3μg/L,结果令人满意。     

集成芯片毛细管电泳电化学检测系统

研制了一种新颖的集成芯片毛细管电泳电化学检测装置。此装置基于柱末安培检测法，将检测池集成芯片上，以自制的30μmPt微盘电极为工作电极，在几十年秒钟内实现了多巴胺、5－羟色胺和肾上腺素三种神经递质的快速分离检测。     

蜂蜜含糖量的高效毛细管电泳测定研究

利用自制的毛细管电泳－电化学安培检测装置，以铜电极为工作电极，在氢氧化钠介质中，分别对２种蜂蜜样品中的糖类化合物进行分离检测，结果满意。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

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.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

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.