Quantitation of glucosamine sulfate in plasma by HPLC-MS/MS after administration of powder for oral solution formulation

A rapid method for the quantification of glucosamine in human plasma using high‐performance liquid chromatography coupled to tandem mass spectrometry was developed and validated. The sample preparation includes a simple deproteinization step, using d ‐[1‐¹³C] glucosamine hydrochloride as an internal standard. Chromatographic separation was performed on an ACE Ciano column using isocratic elution with acetonitrile and aqueous 2 mm ammonium acetate containing 0.025% formic acid (80:20). Selected reaction monitoring was performed using the transitions m/z 180.1 → m/z 72.1 and m/z 181.0 → m/z 74.6 to quantify glucosamine and internal standard, respectively. The method was validated and proved to be linear, accurate and precise over the range 50–5000 ng/mL of glucosamine. Recovery rates higher than 90% were obtained for both glucosamine and internal standard. No matrix effect was detected in the samples. The validated method was successfully applied to a pharmacokinetic study after oral administration of a powder for oral solution formulation containing glucosamine sulfate. Copyright © 2011 John Wiley & Sons, Ltd.     

Low intensity infrared laser effects on Escherichia coli cultures and plasmid DNA

Biostimulative effect of low intensity laser in tissues has been described on a photobiological basis and clinical protocols are recommended for treatment of various diseases. The aim of this work was to evaluate effects of laser exposure on the survival of Escherichia coli cultures and plasmid topological forms. Escherichia coli cultures and plasmids were exposed to infrared laser to study bacterial survival and electrophoretic profile, respectively. Data indicate low intensity infrared laser: (i) had no effect on E. coli wild type, endonuclease IV, exonuclease III, formamidopyrimidine DNA glycosylase/MutM protein and endonuclease III deficient cultures, but decreased the survival of E. coli UvrA protein deficient cultures; (ii) there was no alteration in the electrophoretic profile of plasmids. Exposure to low intensity infrared laser decreases survival of Escherichia coli cultures deficient in nucleotide excision repair of DNA and this effect could depend on fluences, wavelength and tissues conditions.     

Lectin from Canavalia brasiliensis seeds (ConBr) is a valuable biotechnological tool to stimulate the growth of Rhizobium tropici in vitro

To study the interactions between a Rhizobium tropici strain and lectins isolated from the seeds of Canavalia ensiformis (ConA) and Canavalia brasiliensis (ConBr), a lectin fluorescence assay was performed. In addition, an experiment was designed to evaluate the effect of the two lectins on bacterial growth. Both lectins were found to bind to R. tropici cells, but the interactions were inhibited by D-mannose. Interestingly, only ConBr stimulated bacterial growth in proportion to the concentrations used (15.6-500 μg/mL), and the bacterial growth stimulation was inhibited by D-mannose as well. Structure/Function analyses by bioinformatics were carried out to evaluate the volume and carbohydrate recognition domain (CRD) configuration of ConA and ConBr. The difference of spatial arrangement and volume of CRD may indicate the variation between biological activities of both lectins. The results suggest that ConBr could be a promising tool for studies focusing on the interactions between rhizobia and host plants.     

Retinyl palmitate polymeric nanocapsules as carriers of bioactives

Nanocapsules containing poly(d,l-lactide) shell and retinyl palmitate core have been prepared by the pre-formed polymer interfacial deposition method. Dynamic light scattering measurements yielded an average hydrodynamic diameter of ～220nm and a polydispersity index of ～0.12. Small-angle neutron scattering experiments revealed the presence of two populations of nanocapsules of core diameters ～192 and 65nm. Freeze fracture transmission electron microscopy showed a polydisperse population of nanocapsules (NC), with a poly(d,l-lactide) shell thickness between 11 and 3nm. For comparison purposes, nanoemulsions (NE, no polymer) and nanospheres (NS, polymer matrix) were also prepared. Each type of nanoparticles exhibited a different morphology (when examined by electron microscopy), in particular NC showed deformability by capillary adhesion. All three types of nanoparticles successfully encapsulated the poorly water-soluble molecules baicalein and benzophenone-3. The thermal behavior of the various nanoparticles was different to a physical mixture of its individual components. Cytotoxicity and phototoxicity assays, performed in human keratinocytes (HaCaT) and murine fibroblasts (BALB/c 3T3), showed that the NC were only cytotoxic at high concentrations. In vitro release studies of benzophenone-3, by the dialysis bag method using NC and NS, showed a sustained release; however, permeation studies using plastic surgery human abdominal skin in Franz diffusion cells showed that a higher amount of benzophenone-3 from NC penetrated into the skin, most probably due to the deformable nature of these nanoparticles.     

Carbon Nanotube Based Sensor for Simultaneous Determination of Acetaminophen and Ascorbic Acid Exploiting Multiple Response Optimization and Measures in the Presence of Surfactant

A simple procedure for the simultaneous determination of acetaminophen (AC) and ascorbic acid (AA) by differential pulse voltammetry (DPV) using a carbon nanotube paste electrode exploiting measures in cetylpyridinium bromide (CPB) medium is described. Under the best instrumental parameters of DPV, optimized by means of factorial design, the calibration plots in the range 100.0–700.0 µmol L^?1 (r=0.993) and 39.4–146.3 µmol L^?1 (r=0.995) with limits of detection of 7.1 and 2.1 µmol L^?1, were achieved for AA and AC, respectively. The developed method was successfully applied for the AC and AA determination in pharmaceutical formulations, whose accuracy was attested by comparison with HPLC method.     

Flow regimes in wet conical spouted beds using glass bead mixtures

Using a high-viscosity Newtonian fluid, glycerol, an experimental investigation was carried out to evaluate the stable spouting regime in conical spouted beds using four particle mixtures： a reference （monoparticles）, a binary mixture, two ternary mixtures with flat and Gaussian distributions respectively. The mixtures were selected for particle diameters （dp） ranging from 1.09 to 4.98 mm and particle diameter ratios （dpL/dps） ranging from 1.98 to 4.0. Experimental data show that pressure fluctuation signals of the bed, as indicated by changes in their standard deviations, provide suitable information to identify the range of operational conditions for stable spouting. However, the analysis of skewness of curves of pressure fluctuation as a function of air velocity appears not sufficient to identify a particular flow regime. For glycerol in the spouting regime, the standard deviation is noted to increase with increasing glycerol concentration due to the growth of interparticle forces. The implications of these research findings on the drying of suspensions in conical spouted beds using glass bead mixtures are also discussed.     

Potentiometric determination of acids and bases using a silica gel based carbon-epoxy indicator electrode

The construction and the application of a silica gel based carbon-epoxy indicator electrode for the potentiometric determination of acids and bases are described. The effect of composition of silica gel and carbon-epoxy, slope (mV/pH), linear response (pH range) and the use for acid-base titrations were investigated. The data obtained for the acid-base titrations were compared with those obtained using a glass electrode in the same conditions. The electrode showed a linear response in the pH 2 to 13 range with a slope of –40.5 ± 0.4 mV/pH (at 25 °C) and a response time of less than 15 s. The lifetime of the electrode was higher than one year (over 6000 determinations) with a decrease of only 5% of the initial potentiometric response. The silica gel based carbon-epoxy electrode showed excellent results in the end-point indication potentiometric titrations in determination of acids and bases. The miniaturization of the proposed electrode for flow injection analysis was investigated. Received: 11 August 1999 / Revised: 4 October 1999 / Accepted: 7 October 1999     

Green Extraction Techniques as Advanced Sample Preparation Approaches in Biological,Food, and Environmental Matrices: A Review

Green extraction techniques (GreETs) emerged in the last decade as greener and sustainable alternatives to classical sample preparation procedures aiming to improve the selectivity and sensitivity of analytical methods, simultaneously reducing the deleterious side effects of classical extraction techniques (CETs) for both the operator and the environment. The implementation of improved processes that overcome the main constraints of classical methods in terms of efficiency and ability to minimize or eliminate the use and generation of harmful substances will promote more efficient use of energy and resources in close association with the principles supporting the concept of green chemistry. The current review aims to update the state of the art of some cutting-edge GreETs developed and implemented in recent years focusing on the improvement of the main analytical features, practical aspects, and relevant applications in the biological, food, and environmental fields. Approaches to improve and accelerate the extraction efficiency and to lower solvent consumption, including sorbent-based techniques, such as solid-phase microextraction (SPME) and fabric-phase sorbent extraction (FPSE), and solvent-based techniques (μQuEChERS; micro quick, easy, cheap, effective, rugged, and safe), ultrasound-assisted extraction (UAE), and microwave-assisted extraction (MAE), in addition to supercritical fluid extraction (SFE) and pressurized solvent extraction (PSE), are highlighted.     

Determination of uranium and thorium in sediments from Cananéia-Iguape system,Brazil

Journal of Radioanalytical and Nuclear Chemistry - The Cananéia-Iguape system is a complex of lagoon and estuarine channels located in the south of state of São Paulo. This system...