Search results for "PRECIPITATION"

Determination of 3-(4′-methylbenzylidene)camphor and its metabolite 3-(4′-carboxybenzylidene)camphor in human semen by solid-phase extraction and liq…

2015

An analytical method for the determination of the controversial UV filter 3-(4′-methylbenzylidene)camphor (MBC) and its metabolite 3-(4′-carboxybenzylidene)camphor (CBC) in human semen is presented. The method is based on the simultaneous hydrolysis of phase II conjugates and protein precipitation, followed by solid-phase extraction (SPE) and liquid chromatography tandem mass spectrometry (LC-MS/MS) detection. The proposed method was validated by analyzing spiked analyte-free human semen samples. Matrix-matched calibration using an analyte-free semen pool was employed. Satisfactory recoveries (92–114%) were obtained using this calibration methodology, thus showing the accuracy of the propos…

Quantitation of talinolol in rat plasma by LC-MS-MS.

2010

The aim of this study was to develop and validate an assay based on liquid chromatography-tandem mass spectrometry to quantitate talinolol in rat plasma. After a simple protein precipitation step, separation was performed by reversed-phase liquid chromatography using gradient elution with acetonitrile-water-formic acid. Electrospray ionization in the positive ion mode with multiple reaction monitoring was used to analyze talinolol employing propranolol as internal standard. The calibration curve for talinolol was linear over the concentration range 1-250 ng/mL with a correlation coefficient0.995. The method was sensitive (limit of quantitation, 1 ng/mL) and had acceptable accuracy (85-115% …

Expression and purification of polyhistidine-tagged rotavirus NSP4 proteins in insect cells

2003

The rotavirus nonstructural NSP4 protein, a transmembrane endoplasmic reticulum-specific glycoprotein, has been described as the first viral enterotoxin. Purified NSP4 or a peptide corresponding to NSP4 residues 114-135 induces diarrhea in young mice. NSP4 has a membrane-destabilizing activity and causes an increase in intracellular calcium levels and chloride secretion by a calcium-dependent signalling pathway in eucaryotic cells. In this study, four recombinant baculoviruses were generated expressing the rotavirus NSP4 glycoprotein from the human strains Wa and Ito, the porcine strain OSU, and the simian strain SA11, which belong to two different NSP4 genotypes, A and B. The recombinant g…

Purification of Large Cytosolic Proteases for In Vitro Assays: 20S and 26S Proteasomes

2012

Proteasomes are the main cytosolic proteases responsible for generating peptides for antigen processing and presentation in the MHC (major histocompatibility complex) class-I pathway. Purified 20S and 26S proteasomes have been widely used to study both specificity and efficiency of antigen processing. Here, we describe the purification of active human 20S and 26S proteasomes from human erythrocytes by DEAE-ion exchange chromatography, ammonium sulfate precipitation, glycerol density gradient centrifugation, and Superose-6 size exclusion chromatography and their characterization using fluorogenic substrates and specific inhibitors.

Photocatalytic behaviour of metal-loaded TiO2 aqueous dispersions and films

2007

Abstract Titanium dioxide nanoparticles loaded with Ce, Co, Eu, Sm, W and Yb species were prepared by coprecipitation in mild conditions using TiCl 4 as precursor with the aim to enhance the photocatalytic activity, especially under visible light irradiation. The photocatalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), specific surface area (SSA) determination and UV–Vis diffuse reflectance spectroscopy. The photocatalytic activity of the powders of pure and loaded TiO 2 was investigated by employing the photodegradation of 4-nitrophenol as probe reaction in a liquid–solid system. Loading with suitable amounts of W, Co and Sm resulted in a significan…

Synthesis of hydrophilic polymers in supercritical carbon dioxide in the presence of a siloxane-based macromonomer surfactant: Heterogeneous polymeri…

2003

Batch free radical polymerization of 1-vinyl-2-pyrrolidone (VP) in super- critical carbon dioxide (scCO2) was studied in the presence of a reactive polysiloxane surfactant (PDMS-mMA). Phase behavior investigation showed that when the initial concentration of the surface active macromonomer was higher than 2.5% w/w with respect to the monomer, the reaction mixture, in the absence of efficient stirring, was initially opaque to the visible light, and it slowly turned to an orange tint. Polymeriza- tion experiments carried out with surfactant concentration higher than the aforemen- tioned value proceeded with a fast kinetics, and led to the formation of spherical nanoparticles with almost quant…

Dispersion polymerization of methyl methacrylate in supercritical carbon dioxide stabilized with poly(ethylene glycol)-b-perfluoroalkyl compounds

2004

Abstract In this work selected components of an easily synthesible class of poly(ethylene glycol)-perfluoroalkyl block compounds were tested as stabilizers for the dispersion polymerization of methyl methacrylate in scCO 2 . As already observed in the case of different block surfactants the anchor soluble balance (ASB) of the stabilizer is the crucial parameter affecting the efficacy of the stabilization and the kinetics of the polymerization process. When stabilizers with appropriate ASB were used, high molecular weight poly(methyl methacrylate) was synthesized under the form of microspherical polymer particles with yields ranging up to 80%. In these experiments the occurrence of a gel-eff…

Liquid-Crystalline Colloidal Particles

2004

Here we report about the synthesis of colloidal particles of nematic and smectic liquid-crystalline polymers. For this purpose mesogen-containing acrylate monomers were synthesized and polymerized in a special modification of a precipitation polymerization called dispection polymerization. By variation of the polymerization conditions colloidal particles of different size and polydispersity could be obtained including very narrowly distributed samples in optimized batches. On azobenzene-containing colloidal particles switching experiments with polarized light were performed. It could be observed that the nematic director of the mesogens within the colloidal particles can be rotated due to t…

On the interlayer spacing collaps of the Cloisite® 30B organoclay

2011

The natural hydrous sodium silicates from the northern bank of Lake Chad : occurrence, petrology and genesis

2005

Abstract Hydrous sodium silicates sometimes associated with zeolites, form in an alkaline environment, in which there is a high concentration of dissolved silica. Such an environment existed during the Holocene in N'Guigmi interdunal depressions (Lake Chad), which led to the precipitation of various types of hydrous sodium silicates, including magadiite, kenyaite, and zeolites. Scanning electron and optical microscope observations allow several microstructures to be distinguished. These microstructures result from either precipitation sequences or a transformation along a diagenetic gradient. New petrological, microstructural and geochemical data confirm the transformation of magadiite into…