The use of solid sorbents for direct accumulation of organic compounds from water matrices–a review of solid-phase extraction techniques

The main principles of solid-phase extraction techniques are reviewed in this paper. Various solid sorbents can be used as a suitable trap for direct accumulation of organic compounds from aqueous solutions. The trapped analytes can be desorbed by elution with suitably chosen liquid phases. These preconcentration procedures can be considered as low performance liquid chromatography and the efficiency of the procedure can thus be related to the retention characteristics of the preconcentration column. The main sorbents used for trace enrichment purposes are also reviewed. Besides, the concise methodology, sample storage, and automation are discussed. The advantages of solid phase extraction as compared to liquid-liquid extraction are given as well as some drawbacks of this method.     

The comparison of geometric and electronic properties of molecular surfaces by neural networks: Application to the analysis of corticosteroid-binding globulin activity of steroids

Summary It is shown how a self-organizing neural network such as the one introduced by Kohonen can be used to analyze features of molecular surfaces, such as shape and the molecular electrostatic potential. On the one hand, two-dimensional maps of molecular surface properties can be generated and used for the comparison of a set of molecules. On the other hand, the surface geometry of one molecule can be stored in a network and this network can be used as a template for the analysis of the shape of various other molecules. The application of these techniques to a series of steroids exhibiting a range of binding activities to the corticosteroid-binding globulin receptor allows one to pinpoint the essential features necessary for biological activity.     

Gravimetric determination of cobalt and nickel,and their separations from copper with n-benzoylphenylhydroxylamine

N-Benzoylphenylhydroxylamine can be used for the gravimetric determination of cobalt and nickel. The precipitates can be weighed as such, or ignited and weighed as cobalt sulphate or nickclous oxide. Cobalt or nickel can be separated from copper with the reagent.     

PSt-g-PEO两亲接枝共聚物溶液的性质

两亲共聚物是指分子结构中同时具有对两种相结构都有亲和性的聚合物,一般指分子结构中同时含有亲油和亲水基团的共聚物,研究两亲共聚物在选择性溶剂中的形态及聚集态结构,对于其作为表面活性剂,增溶剂,生物医药材料,以及固体微胶束的研究都具有重要的理论和实际意义。[1-3]／     

噻吩光电化学聚合的研究

噻吩在水溶液中先经低聚反应,生成的低聚合物再在阳极氧化成膜,光照可促进低聚合物的形成,使噻吩在Pt、Au基低上选择性地进行光电聚合。即在低于噻吩电聚合电位下,形成明显光照点的聚噻吩膜。     

Improvements in loop atomic absorption spectrometry by application of an iridium loop and a ceramic collection tube

Atomic absorption spectrometry with a metal loop for sample introduction into the flame can be improved by substituting indium for platinum as the loop material. Because of the higher melting point of iridium, elements such as silver, copper and manganese can be readily determined as well as more volatile elements. When a ceramic collection tube is used, limits of detection can be improved further.     

电喷雾质谱在寡糖序列分析中的应用

选取具有不同结构特征的N-糖链、硫酸软骨素寡糖、人乳寡糖以及海洋来源的壳寡糖、褐藻胶寡糖、卡拉胶寡糖和硫酸岩藻寡糖等,对电喷雾质谱在寡糖的主链序列、分支位点、硫酸基取代位置确定、单糖组成和聚合度分析等方面的应用技术及碎片离子的断裂规律进行了总结.根据相邻同类碎片离子之间的质荷比差值可初步判断寡糖的单糖组成类型;通过与色谱分离技术联用或衍生化方法可提高寡糖的分辨率和离子化效率,并测得寡糖的分子量及聚合度;借助串联质谱及对寡糖还原端的特异性标记,可获得寡糖的还原端残基和部分序列信息;根据寡糖产生的特征碎片离子及其丰度大小可判断残基的特定位置和类型.另外,寡糖的分支通常作为一个整体发生糖苷键断裂或产生D离子,据此可判断分支点的位置;根据硫酸寡糖产生的特异性跨环断裂碎片,可以确定硫酸基的连接位置.这些规律和方法的总结为未知寡糖的结构和序列的分析提供了启发和指导.     

Controlled potential electrolytic determination of copper in lead and tin-base alloys

In lead-base alloys, copper can be determined by a single controlled-potential electrolysis if less than 1.5% of antimony is present, otherwise, the deposit must be dissolved and re-electrolyzed Iron tends to inhibit the co-deposition of antimony in tin-base alloys, copper and lead can be determined successively. The sample weight is 5 g; percentages as low as 0.2% can be determined.     

Regio‐ and Stereoselective Modification of Chiral α‐Amino Ketones by Pd‐Catalyzed Allylic Alkylation

Chiral α‐amino ketones are excellent nucleophiles for stereoselective palladium‐catalyzed allylic alkylations. Both chiral as well as achiral allylic substrates can be applied, while the stereochemical outcome of the reaction is controlled by the chiral ketone enolate. The substituted amino ketones formed can be reduced stereoselectively, and up to five consecutive stereogenic centers can be obtained. This approach can be used for the synthesis of highly substituted piperidine derivatives.     

Ultrasensitive quantification of mature microRNAs by real-time PCR based on ligation of a ribonucleotide-modified DNA probe

It was first demonstrated that the DNA probe modified with ribonucleotides can be efficiently ligated by using miRNA as the template. With PCR amplification of the ligated DNA probe, as low as 0.2 fM target miRNAs can be detected with high specificity.     

New ammonia equivalents for the Pd-catalyzed amination of aryl halides

[reaction: see text]. LiN(SiMe3)2, Ph3SiNH2, and LiNH2 can be be used as ammonia equivalents for the Pd-catalyzed coupling of aryl halides. Using these amine derivatives, simple anilines, including ortho-substituted ones, as well as di- and triarylamines can be readily prepared.     

Stereoselective synthesis of beta-substituted phenylalanine-beta-phenylisoserine-derived tripeptides using N-cinnamoyl-L-proline as template: synthesis of structural analogues of HIV protease inhibitors

N-Cinnamoyl-L-proline can be used as a template on which beta-substituted phenylalanine and beta-phenylisoserine residues can be synthesized leading to tripeptide derivatives as structural analogues of HIV protease inhibitors.     

An efficient method for the debutylation of o-and p-t-butylphenols and for the hydrolysis of aryl acetates : [Protective group; quinones]

t-Butyl groups can be removed from mono-, di-, or tri-t-butylphenols by refluxing with 70% trifluoroacetic acid. In the same way sterically hindered as well as unhindered aryl acetates can be hydrolysed.     

Application of a large assembly of microelectrodes to the study of cytochrome-c and other redox proteins

A novel microelectrode assembly containing more than 1000 carbon microdisks has been used to study the interfacial electron transfer kinetics of cytochrome c and several other redox proteins. It is demonstrated that near-steady-state current–voltage curves can be obtained without solution stirring, and without significant mains interference or capacitive charging currents. In addition, it is demonstrated that concentrations of redox proteins as low as 1 μM can be detected in solution. Finally, it is shown that the surfaces of carbon microdisk assemblies can be successfully coated with thin films of poly(ester sulfonic acid), which allows reactants to be studied in a membrane-like environment.     

Indirect Electroorganic Syntheses—A Modern Chapter of Organic Electrochemistry [New Synthetic Methods (59)]

The electrochemical formation and regeneration of redox agents for organic syntheses (indirect electrolysis) widens the potential of electrochemistry, as higher or totally different selectivities can often be obtained while at the same time the energy input can be lowered significantly. Higher current densities can also be obtained by preventing otherwise often encountered electrode inhibition. New types of redox catalysts can be formed in-situ and can be regenerated after reaction with the substrates. This principle is of increasing importance also for the application of already known redox agents with regard to environmental protection, since large amounts of a product can be generated in a closed circuit using only relatively small amounts of the redox reagent. Consequently the operation of such a process can be greatly simplified, and the release of ecologically objectionable spent reagents into the environment can be prevented. The broad spectrum of redox catalysts currently in use includes, inter alia, metal salts in very low or high oxidation states, halogens in various oxidation states, and, in particular, a wide variety of transition-metal complexes. A great deal of progress has recently been made in the application of organic electron transfer agents, since compounds have been found that are sufficiently stable in both the reduced as well as the oxidized state.     

Synthesis and supramolecular characterization of a novel class of glycopyranosyl-containing amphiphiles

A novel class of glycopeptidolipids is described, which potentially can be used as a novel antigen-delivery system. The compounds have been prepared by a combination of solid-supported and solution-based methods. The use of the orthogonally protected FmocLysDde derivative provided an opportunity to incorporate two different types lipids. It was found that the model compound 1 forms aggregates in aqueous media which can be described as rod or tubelike structures. The aggregates can be stabilized by topotactic photopolymerization. Studies on the structural analogues 2-5 revealed the effect of the carbohydrate, peptide, and lipid moiety on the aggregation properties. It is concluded that none of the structure elements can lay claim to be exclusively important for the formation of highly organized aggregates such as tubes, fibers, or helical ribbons from 1, but the presence of all of these structural elements afforded the most uniformly shaped extended structures.     

On the use of alumina in HPLC with aqueous mobile phases at extreme pH

Summary The applicability of alumina as a stationary phase in liquid chromatography is considered. Despite the presence of hydroxyl groups on wetted alumina, chemical modification with silanes by analogy to silica is not successful. Although depolarisation can be achieved with hexamethyldisilazane, the product is not stable to hydrolysis in aqueous media. The use of alumina as an ion-exchanger is more promising, especially because alumina appears to be stable over a very broad pH range. As a result of its amphoteric character alumina can be used either as an anion-exchanger or as a cation-exchanger. The latter possibility is more profitable in alkaline solvents and allows the separation of strongly basic compounds at pH values as high as 12. Retention can be controlled by judicious choice of ionic strength, counter ion and pH.     

Thin-layer chromatographic determination of aldehydes encountered in foods as dimethones, octahydroxantheines and barbiturates

Aldehydes in foods can conveniently be characterized and determined by thin-layer chromatography (TLC) after converting them into their dimethones. For further confirmation the dimethones can be cyclized on the TLC plates or in solution to give octahydroxanthenes. Aldehydes also can be determined as their barbiturates. The aldehydes could be determined as dimethones and octahydroxanthenes in amounts up to 5 micrograms and as barbiturates in amounts up to 7.5 micrograms at their UV maxima.     

Chemical modification of polymeric hydrocarbons

Although polymeric hydrocarbons (PCH) carry no functions, they can be modified in many ways. Unsaturated PCH undergo addition reactions as hydrogenation, halogenation, epoxidation and thiol addition. Saturated PCH can be substituted with various functions, notably halogen and chlorosulfonyl groups. All PCH can be modified, by a grafting mechanism, with functional monomers as maleic anhydride. Some modified PCH play a major role in multiphase systems as blends, rubber-modified thermoplastics and thermoplastic elastomers. Attractive grafting procedures involve in-situ grafting in PCH/monomer solutions and during reactive blending processes.