Immunomagnetic separation and detection of Salmonella cells using newly designed carriers

A new method for simultaneous determination of alkoxyethanols (2-methoxyethanol, 2-ethoxyethanol, 2-isopropoxyethanol, and 2-butoxyethanol) by high-performance liquid chromatography (HPLC) with fluorescence detection has been developed. The alkoxyethanols and an internal standard (2-phenoxyethanol) were derivatized by treatment with 1-anthroylnitrile to give the anthroyl esters. The esterification was completed in 30 min in the presence of quinuclidine as base catalyst at room temperature. After stopping the reaction, an aliquot of the final solution was injected into the HPLC. The resulting anthroyl esters of the alkoxyethanols and the internal standard were separated on a C18 reversed-phase column with acetonitrile-water-acetic acid (65:35:0.1, v/v) as the mobile phase and detected fluorimetrically at excitation and emission wavelengths of 360 nm and 460 nm, respectively. The detection limits of the derivatives as alkoxyethanols at a signal-to-noise ratio of 3 were in the range of 1-3 pg per injection. The minimal amounts of alkoxyethanols derivatized in the reaction mixture for derivatization to determine the limits of detection were approximately 0.5 ng. This HPLC method was applied to the determination of some of alkoxyethanols in the air of the workplace where the thinner containing alkoxyethanols was used for painting.     

Experimental-Untersuchungen über das periodische Gesetz. I. Theil

Ohne ZusammenfassungDer wesentliche Inhalt dieser Abhandlung wurde der kaiserl. Akademie in einem versiegelten Schreiben am 14. Februar 1889, unter dem Titel: Über eine Anomalie des periodischen Systems vorgelegt.     

Volumetrische Bestimmung des Tellurs

Ohne ZusammenfassungAkadem. Anzeiger Nr. XVIII, 1890.     

Volumetrische Bestimmung des Tellurs,eine maassanalytische Studie,I. Theil

Ohne Zusammenfassung     

Accuracy and sensitivity of the determination of rate constants of interconversion in achiral and chiral environments by dynamic enantioselective electrophoresis

The method for determination of rate constants of interconversion of enantiomers in chiral and achiral environments of a dynamic enantioseparation system was investigated in order to reveal its accuracy, sensitivity and robustness. Two significantly different enantioseparation systems were selected, one with a single (well-defined) chiral selector (CS) and the second with a mixture of CSs, and the rate constants of interconversion for these two systems were compared statistically. While the rate constants of interconversion in the chiral environment were found to be significantly different, the rate constants in achiral environment were confirmed to be statistically the same. The accuracy of the method was independent of experimental conditions. Influence of a CS and temperature on the rate of interconversion were discussed within the scope of determined thermodynamic parameters and statistical evaluation. A certain temperature may exist at which two different types of CSs influence the rate of interconversion equally while the extent of their influence may largely differ at other temperatures.     

Determination of neopterin, kynurenine, tryptophan and creatinine in human serum by high throuput HPLC

A new HPLC method for simultaneous determination of neopterin, creatinine, kynurenine and tryptophan in human serum was developed and validated. Monolithic stationary phase's technology (two monolithic columns RP-18e were connected with guard monolithic cartridge 4.6 mm × 50 mm + 3.0 mm × 100 mm and 4.6 × 10 mm) and special auto sampler for micro titration plates (samples are storage in dark cooled place protected against evaporation) were combined with easy sample preparation step. As mobile phase 15 mmol/L phosphate buffer at pH 4.50 was used. Neopterin and tryptophan were detected using fluorescent detection and kynurenine and creatinine were detected by diode-array detection. This method may be suitable for large sequences of samples in clinical research and routine practice.     

Mn2+ complexes with 12-membered pyridine based macrocycles bearing carboxylate or phosphonate pendant arm: crystallographic, thermodynamic, kinetic, redox, and 1H/17O relaxation studies

Mn(2+) complexes represent an alternative to Gd(3+) chelates which are widely used contrast agents in magnetic resonance imaging. In this perspective, we investigated the Mn(2+) complexes of two 12-membered, pyridine-containing macrocyclic ligands bearing one pendant arm with a carboxylic acid (HL(1), 6-carboxymethyl-3,6,9,15-tetraazabicyclo[9.3.1] pentadeca-1(15),11,13-triene) or a phosphonic acid function (H(2)L(2), 6-dihydroxyphosphorylmethyl-3,6,9,15-tetraazabicyclo[9.3.1]pentadeca-1(15),11,13-triene). Both ligands were synthesized using nosyl or tosyl amino-protecting groups (starting from diethylenetriamine or tosylaziridine). The X-ray crystal structures confirmed a coordination number of 6 for Mn(2+) in their complexes. In aqueous solution, these pentadentate ligands allow one free coordination site for a water molecule. Potentiometric titration data indicated a higher basicity for H(2)L(2) than that for HL(1), related to the electron-donating effect of the negatively charged phosphonate group. According to the protonation sequence determined by (1)H and (31)P pH-NMR titrations, the first two protons are attached to macrocyclic amino groups whereas the subsequent protonation steps occur on the pendant arm. Both ligands form thermodynamically stable complexes with Mn(2+), with full complexation at physiological pH and 1:1 metal to ligand ratio. The kinetic inertness was studied via reaction with excess of Zn(2+) under various pHs. The dissociation of MnL(2) is instantaneous (at pH 6). For MnL(1), the dissociation is very fast (k(obs) = 1-12 × 10(3) s(-1)), much faster than that for MnDOTA, MnNOTA, or the Mn(2+) complex of the 15-membered analogue. It proceeds exclusively via the dissociation of the monoprotonated complex, without any influence of Zn(2+). In aqueous solution, both complexes are air-sensitive leading to Mn(3+) species, as evidenced by UV-vis and (1)H NMRD measurements and X-ray crystallography. Cyclic voltammetry gave low oxidation peak potentials (E(ox) = 0.73 V for MnL(1) and E(ox) = 0.68 V for MnL(2)), in accordance with air-oxidation. The parameters governing the relaxivity of the Mn(2+) complexes were determined from variable-temperature (17)O NMR and (1)H NMRD data. The water exchange is extremely fast, k(ex) = 3.03 and 1.77 × 10(9) s(-1) for MnL(1) and MnL(2), respectively. Variable-pressure (17)O NMR measurements have been performed to assess the water exchange mechanism on MnL(1) and MnL(2) as well as on other Mn(2+) complexes. The negative activation volumes for both MnL(1) and MnL(2) complexes confirmed an associative mechanism of the water exchange as expected for a hexacoordinated Mn(2+) ion. The hydration number of q = 1 was confirmed for both complexes by (17)O chemical shifts. A relaxometric titration with phosphate, carbonate or citrate excluded the replacement of the coordinated water molecule by these small endogenous anions.     

A local convergence proof for the iterative aggregation method

The iterative aggregation method for the solution of a system of linear algebraic equations x = Ax + b, where A ≥ 0, b ≥ 0, s > 0, and s ′ A < s ′, is proved to be locally convergent. It is shown that the method can be considered a consistent nonstationary iterative method, where the iteration matrix depends on the current iterate, and that some norm of the iteration matrix is less than one in the vicinity of the solution.