Preparation and evaluation of sulfur-containing metal chelators

With a view to probe the structure and function of G-protein coupled receptors the synthesis of functionalized 8-mercaptoquinoline derivatives and 2-(2-pyridyl)thiophenol was achieved. A fluorescence-based method for determining the affinity of these metal chelators toward zinc ions was developed.     

Synthesis and evaluation of novel pyridine based PLG tripeptidomimetics

Analogues of the pyridine based PLG (Pro-Leu-Gly-NH(2)) peptidomimetic were synthesized and evaluated as dopamine modulating agents. Modifications in the position corresponding to the leucine side chain in PLG afforded derivatives , and , substituted with H, Me and Bn instead of the isobutyl group, respectively. Changes in the proline residue produced derivative , substituted with a symmetrical piperidine ring instead of the pyrrolidine ring and , in which the pyrrolidine ring is connected to the pyridine ring via a hydroxymethyl group instead of a keto function. The peptidomimetics were tested for their ability to enhance the maximal effect of N-propylapomorphine (NPA) at dopamine D2 receptors in the functional cell-based R-SAT assay. Compounds , , and , produced a statistically significant increase in the maximal NPA response at 10 nM (117 +/- 6%, 118 +/- 6%, and 116 +/- 3%, respectively), which is similar to the effect of PLG in this assay, whereas was able to potentiate the response to a similar extent at 1 nM concentration (115 +/- 5%). All derivatives produced a bell-shaped dose-response curve and none of the compounds were active at the D2 receptor alone, which indicates that the mechanism behind the activity of both the pyridine based mimetics and PLG is the same. Interestingly, l-Pro-d-Leu-Gly-NH(2) was found to be more potent than PLG and produced a 119 +/- 1% increase in the NPA response at 1 nM.     

Erratum to: Inter-laboratory exercise with an aim to compare methods for 90Sr and 239,240Pu determination in environmental soil samples

Journal of Radioanalytical and Nuclear Chemistry - In the original article, the LOD assigned to method Sr-B in Table 1 was published incorrectly as 24 Bq/kg, the correct LOD for...     

High-throughput synthesis and analysis of acylated cyanohydrins

The yields and optical purities of products obtained from chiral Lewis acid/Lewis base-catalysed additions of alpha-ketonitriles to prochiral aldehydes could be accurately determined by an enzymatic method. The amount of remaining aldehyde was determined after its reduction to an alcohol, whilst the two product enantiomers were analysed after subsequent hydrolysis first by the (S)-selective Candida antarctica lipase B and then by the unselective pig liver esterase. The method could be used for analysis of products obtained from a number of aromatic aldehydes and aliphatic ketonitriles. Microreactor technology was successfully combined with high-throughput analysis for efficient catalyst optimization.     

A fully robust PARAFAC method for analyzing fluorescence data

Parallel factor analysis (PARAFAC) is a widespread method for modeling fluorescence data by means of an alternating least squares procedure. Consequently, the PARAFAC estimates are highly influenced by outlying excitation–emission landscapes (EEM) and element‐wise outliers, like for example Raman and Rayleigh scatter. Recently, a robust PARAFAC method that circumvents the harmful effects of outlying samples has been developed. For removing the scatter effects on the final PARAFAC model, different techniques exist. Newly, an automated scatter identification tool has been constructed. However, there still exists no robust method for handling fluorescence data encountering both outlying EEM landscapes and scatter. In this paper, we present an iterative algorithm where the robust PARAFAC method and the scatter identification tool are alternately performed. A fully automated robust PARAFAC method is obtained in that way. The method is assessed by means of simulations and a laboratory‐made data set. Copyright © 2009 John Wiley & Sons, Ltd.     

Chemical resistance and cleanability of glazed surfaces

Adhesion of soil on glazed surfaces and their cleanability depends on chemical composition, phase composition, and roughness of the surface. The surface can be glossy consisting mainly of a smooth glassy phase. A matt and rough surface consists of a glassy phase and one or more crystalline phases. The origin and composition of the crystalline phases affect the chemical resistance and the cleanability of the surface. Fifteen experimental glossy and matt glazes were soaked in a slightly alkaline cleaning agent solution. The surfaces were spin-coated with sebum, i.e. a soil component typical for sanitary facilities. After wiping out the soil film in a controlled manner, the surface conditions and the soil left were evaluated with colour measurements, SEM/EDXA and COM. The results show that wollastonite-type crystals in the glaze surfaces were attacked in aqueous solutions containing typical cleaning agents. This corrosion led to significant decrease in the cleanability of the surface. The other crystal types observed, i.e. diopside and quartz crystals were not corroded, and the cleanability of glazes containing only these crystals was not changed in the cleaning agent exposures. Also the glassy phase was found to be attacked in some formulations leading to a somewhat decreased cleanability. The repeated soiling and cleaning procedures indicated that soil is accumulated on rough surfaces and surfaces which were clearly corroded by the cleaning agent.     

Peak alignment and robust principal component analysis of gas chromatograms of fatty acid methyl esters and volatiles

Gas chromatograms of fatty acid methyl esters and of volatile lipid oxidation products from fish lipid extracts are analyzed by multivariate data analysis [principal component analysis (PCA)]. Peak alignment is necessary in order to include all sampled points of the chromatograms in the data set. The ability of robust algorithms to deal with outlier problems, including both sample-wise and element-wise outliers, and the advantages and drawbacks of two robust PCA methods, robust PCA (ROBPCA) and robust singular value decomposition when analysing these GC data were investigated. The results show that the usage of ROPCA is advantageous, compared with traditional PCA, when analysing the entire profile of chromatographic data in cases of sub-optimally aligned data. It also demonstrates how choosing the most robust PCA (sample or element-wise) depends on the type of outliers present in the data set.     

Recoverable resin-supported pyridylamide ligand for microwave-accelerated molybdenum-catalyzed asymmetric allylic alkylations: enantioselective synthesis of baclofen

The syntheses of a series of 4-monosubstituted pyridylamides and a resin-supported pyridylamide are described. The ligands were evaluated in the microwave-accelerated molybdenum-catalyzed asymmetric allylic alkylation. The reaction afforded the product in high yield and with high regio- and enantioselectivity. The heterogeneous ligand could be reused several times with no change in the reaction outcome. The asymmetric allylic alkylation was employed as the key step in the enantioselective synthesis of (R)-baclofen. [reaction: see text]