Kit preparation of153Sm-EDTMP and factors affecting radiochemical purity and stability

A fast kit method was developed for the production of¹⁵³Sm-EDTMP in two steps avoiding the use of nitric acid, evaporation and sterilization of the final solution by autoclave. Methods of analysis for the determination of chemical and radiochemical purity in the radiopharmaceutical solution were established. Factors affecting radiochemical purity and stability of the complex as the molar ratio of EDTMP/Sm, concentration of phosphate buffer and neutralization of EDTMP prior kit preparation were also analyzed. The use of this radiopharmaceutical in rabbits and patients showed selective skeletal uptake.     

Analytical determination of polyphenols in olive oils

The increasing popularity of olive oil is mainly attributed to its high content of oleic acid, which may affect the plasma lipid/lipoprotein profiles, and its richness in phenolic compounds, which act as natural antioxidants and may contribute to the prevention of human disease. An overview of analytical methods for the measurement of polyphenols in olive oil is presented. In principle, the analytical procedure for the determination of individual phenolic compounds in virgin olive oil involves three basic steps: extraction from the oil sample, analytical separation, and quantification. A great number of procedures for the isolation of the polar phenolic fraction of virgin olive oil, utilizing two basic extraction techniques, LLE or SPE, have been included. The reviewed techniques are those based on spectrophotometric methods, as well as analytical separation (gas chromatography (GC), high-performance liquid chromatography (HPLC), and capillary electrophoresis (CE)). Many reports in the literature determine the total amount of phenolic compounds in olive oils by spectrophometric analysis and characterize their phenolic patterns by capillary gas chromatography (CGC) and, mainly, by reverse phase high-performance liquid chromatography (RP-HPLC); however, CE has recently been applied to the analysis of phenolic compound of olive oil and has opened up great expectations, especially because of the higher resolution, reduced sample volume, and analysis duration. CE might represent a good compromise between analysis time and satisfactory characterization for some classes of phenolic compounds of virgin olive oils.     

A general entry to linear, dendritic and branched thiourea-linked glycooligomers as new motifs for phosphate ester recognition in water

A blockwise iterative synthetic strategy for the preparation of linear, dendritic and branched full-carbohydrate architectures has been developed by using sugar azido(carbamate) isothiocyanates as key templates; the presence of intersaccharide thiourea bridges provides anchoring points for hydrogen bond-directed molecular recognition of phosphate esters in water.     

Subminute and sensitive determination of the neurotransmitter serotonin in urine by capillary electrophoresis with laser-induced fluorescence detection

In this work, a sub-minute and sensitive capillary electrophoresis with laser-induced fluorescence (CE-LIF) method was developed for the analysis and quantitation of the neurotransmitter 5-hydroxytryptamine (5-HT) or serotonin in urine. The method involves precolumn derivatization with fluorescein isothiocyanate isomer I (FITC) using an excitation light from an argon ion laser of 488 nm and a 520 nm band pass emission filter. Different variables that affect derivatization (pH, FITC concentration, reaction time and temperature) and separation (buffer concentration, pH, applied voltage and injection time) were studied. The linear dynamic range obtained was between 0 and 188 nM with a detection limit of 16 nm with a RSD between 2 and 9%. The applicability of the proposed method was demonstrated by analysis of 5-HT in human urine, establishing a concentration of 57 nM in control urine. The method was validated by standard-addition methodology.     

Detection of tamoxifen metabolites by GC-MSD

Tamoxifen is an antiestrogen used in the adjuvant endocrine therapy of early breast cancer and malignant breast disorders. It is also used in women with anovulatory infertility caused by its stimulating effect on the secretion of the pituitary gonadotrophic hormones. In males it could increase the endogenous production of androgens. Because of these properties tamoxifen may be misused in some sports to treat the androgens suppression caused by the extensive abuse of anabolic androgenic steroids. A method for identification and confirmation of tamoxifen metabolites is described. Hydroxymetoxytamoxifen is detected in urine by gas chromatography and mass spectrometry in a selective ion monitoring method followed by the routine postrun in the screening of anabolic steroids. Once the hydroxymetoxytamoxifen is detected, confirmation of reported metabolites could be performed with a 5973 mass selective detector in the scan mode after solid-phase extraction by cationic exchange. This study also reports an excretion profile for a single dose of tamoxifen equivalent to 40 mg administrated orally to two males volunteers.     

Regularity of weak solutions to the Monge-Ampère equation

We study the properties of generalized solutions to the Monge-Ampère equation , where the Borel measure satisfies a condition, introduced by Jerison, that is weaker than the doubling property. When , this condition, which we call , admits the possibility of vanishing or becoming infinite. Our analysis extends the regularity theory (due to Caffarelli) available when , which implies that is doubling. The main difference between the case and the case when is bounded between two positive constants is the need to use a variant of the Aleksandrov maximum principle (due to Jerison) and some tools from convex geometry, in particular the Hausdorff metric.

     

High-performance liquid chromatographic determination of furfural and hydroxymethylfurfural in apple juices and concentrates

Summary A rapid and sensitive method for determining 2-furaldehyde (FUR) and 5-hydroxymethyl-2-furaldehyde (HMF) in apple juices and juice concentrates has been developed. The method for FUR and HMF involves the solid-liquid extraction of the juice by using a C-18 cartridge prior to reversed-phase separation with detection at 280 nm. The mobile phase was acetonitrile-water (8/92, v/v) at a flow rate of 1.0 ml/min. Recoveries from apple juices and juice concentrates spiked at different levels ranged from 94.1 to 104.0 (FUR) and 94.5 to 100.5 (HMF). The quantification limit for both, FUR and HMF, was 5 ppb.     

Laser-surface-alloying of the iron based superalloy Incoloy-800H with Al

Laser surface alloying by the powder feed method of the iron based superalloy Incoloy 800H with aluminium has been carried out. The effects of different preparation parameters, like laser scan speed and powder feed rate, on the morphology of the alloyed zone have been investigated. Microstructure and composition have been determined by scanning electron microscopy (SEM), optical microscopy, and x-ray fluorescence spectroscopy. Three different phases with different Al-content have been distinguished. The observed Al-enrichment at the surface, the presence of Ni-Al and Fe-Al intermetallic compounds, and the considerable grain refining of the alloyed zone with respect to the substrate, make this surface modification technique a very good method to improve the corrosion behaviour of the Incoloy 800H super-alloy.     

On the numerical expansion of a second order stochastic process

The utility of the classical Karhunen-Loève expansion of a second order process is limited to its practical derivation, because it depends upon the solution of a Fredholm integral equation associated with it whose kernel is the covariance function of the process. So, in this paper we study two numerical procedures for solving such equations, the Rayleigh-Ritz and the collocation methods, and also essay two different bases of L²-orthogonal functions in order to perform the algorithms, Legendre polynomials and trigonometric functions, on two well-known processes, the Wiener-Lévy process and the Brownian-bridge. The accuracy of the numerical results in relation to the real ones, as well as comparative studies among both procedures are also included.