Development and validation of a fast RP-HPLC method to determine the analogue of the thyroid hormone, 3,5,3 '-triiodothyroacetic acid (TRIAC), in polymeric nanoparticles

The objective of this work was to develop and validate a rapid Reversed-Phase High-Performance Liquid Chromatography method for the quantification of 3,5,3 '-triiodothyroacetic acid (TRIAC) in nanoparticles delivery system prepared in different polymeric matrices. Special attention was given to developing a reliable reproductive technique for the pretreatment of the samples. Chromatographic runs were performed on an Agilent 1200 Series HPLC with a RP Phenomenex (R) Gemini C18 (150 x 4, 6 mm i.d., 5 mu m) column using acetonitrile and triethylamine buffer 0.1% (TEA) (40 : 60 v/v) as a mobile phase in an isocratic elution, pH 5.6 at a flow rate of 1 ml min(-1). TRIAC was detected at a wavelength of 220 nm. The injection volume was 20 mu l and the column temperature was maintained at 35 degrees C. The validation characteristics included accuracy, precision, specificity, linearity, recovery, and robustness. The standard curve was found to have a linear relationship (r(2) - 0.9996) over the analytical range of 5-100 mu g ml(-1) . The detection and quantitation limits were 1.3 and 3.8 mu g ml(-1), respectively. The recovery and loaded TRIAC in colloidal system delivery was nearly 100% and 98%, respectively. The method was successfully applied in polycaprolactone, polyhydroxybutyrate, and polymethylmethacrylate nanoparticles.

Thermal lens and interferometric method for glass transition and thermo physical properties measurements in Nd(2)O(3) doped sodium zincborate glass

In this work the time resolved thermal lens method is combined with interferometric technique, the thermal relaxation calorimetry, photoluminescence and lifetime measurements to determine the thermo physical properties of Nd(2)O(3) doped sodium zincborate glass as a function of temperature up to the glass transition region. Thermal diffusivity, thermal conductivity, fluorescence quantum efficiency, linear thermal expansion coefficient and thermal coefficient of electronic polarizability were determined. In conclusion, the results showed the ability of thermal lens and interferometric methods to perform measurements very close to the phase transition region. These techniques provide absolute values for the measured physical quantities and are advantageous when low scan rates are required. (c) 2008 Optical Society of America

Gibbs random graphs on point processes

Consider a discrete locally finite subset Gamma of R(d) and the cornplete graph (Gamma, E), with vertices Gamma and edges E. We consider Gibbs measures on the set of sub-graphs with vertices Gamma and edges E` subset of E. The Gibbs interaction acts between open edges having a vertex in common. We study percolation properties of the Gibbs distribution of the graph ensemble. The main results concern percolation properties of the open edges in two cases: (a) when Gamma is sampled from a homogeneous Poisson process; and (b) for a fixed Gamma with sufficiently sparse points. (c) 2010 American Institute of Physics. [doi:10.1063/1.3514605]

Method for cadmium and lead longitudinal profiles determination in hair by solid sampling graphite furnace atomic absorption spectrometry

This paper describes methods for the direct determination of Cd and Pb in hair segments (c.a. 5 mm similar to 80 mu g) by solid sampling graphite furnace atomic absorption spectrometry, becoming possible longitudinal profiles in a single strand of hair. To distinguish endogenous and exogenous content. strands of hair were washed by using two different procedures: IAEA protocol (acetone + water + acetone) and the combination of IAEA protocol with HCl washing (acetone + water + acetone + 0.1 mol l(-1) HCl). The concentration of Cd and Pb increased from the root Until the tip of hair washed according to IAEA protocol. However, when the strand of hair was washed using the combination of IAEA protocol and 0.1 mol l(-1) HCl, Cd concentrations decreased in all segments, and Pb concentrations decreased drastically near to the root (5 to 12 mm) and was systematically higher ill the end. The proposed method showed to be useful to assess the temporal variation to Cd and Pb exposure and call be Used for toxicological and environmental investigations. The limits of detection were 2.8 ng g(-1) for Cd and 40 ng g(-1) for Pb. The characteristic masses based oil integrated absorbance were 2.4 pg for Cd and 22 pg for Pb.

Cloud point extraction to avoid interferences by structured background on nickel determination in plant materials by FAAS

An analytical procedure based on microwave-assisted digestion with diluted acid and a double cloud point extraction is proposed for nickel determination in plant materials by flame atomic absorption spectrometry. Extraction in micellar medium was successfully applied for sample clean up, aiming to remove organic species containing phosphorous that caused spectral interferences by structured background attributed to the formation of PO species in the flame. Cloud point extraction of nickel complexes formed with 1,2-thiazolylazo-2-naphthol was explored for pre-concentration, with enrichment factor estimated as 30, detection limit of 5 mu g L(-1) (99.7% confidence level) and linear response up to 80 mu g L(-1). The accuracy of the procedure was evaluated by nickel determinations in reference materials and the results agreed with the certified values at the 95% confidence level.

LEARNING A COMPLEX MOTOR SKILL FROM VIDEO AND POINT-LIGHT DEMONSTRATIONS

The aim of this Study was to compare the learning process of a highly complex ballet skill following demonstrations of point light and video models 16 participants divided into point light and video groups (ns = 8) performed 160 trials of a pirouette equally distributed in blocks of 20 trials alternating periods of demonstration and practice with a retention test a day later Measures of head and trunk oscillation coordination d1 parity from the model and movement time difference showed similarities between video and point light groups ballet experts evaluations indicated superiority of performance in the video over the point light group Results are discussed in terms of the task requirements of dissociation between head and trunk rotations focusing on the hypothesis of sufficiency and higher relevance of information contained in biological motion models applied to learning of complex motor skills

Cloud point extraction and concentration of carbaryl from natural waters

An improved procedure is proposed for determination of the pesticide carbaryl in natural waters based on double cloud point extraction. The clean up step was carried out only with Triton X-114 in alkaline medium in order to avoid the use of toxic organic solvents as well as to minimise waste generation. Cloud point preconcentration of the product of the reaction of the analyte with p-aminophenol and cetyltrimethylammonium bromide was explored to increase sensitivity and improve the detection limit. Linear response was achieved within 10 and 500 mu g L-1 and the apparent molar absorptivity was estimated as 4.6 x 105 L mol-1 cm-1. The detection limit was estimated as 7 mu g L-1 at the 99.7% confidence level and the coefficient of variation was 3.4% (n = 8). Recoveries within 91 and 99% were estimated for carbaryl spiked water samples. The results obtained for natural water samples were in agreement with those achieved by the batch of spectrophotometric procedure at the 95% confidence level. The proposed procedure is then a simple, fast, inexpensive and greener alternative for carbaryl determination.

Neutron Activation Analysis: A Primary (Ratio) Method to Determine SI-Traceable Values of Element Content in Complex Samples

The metrological principles of neutron activation analysis are discussed. It has been demonstrated that this method can provide elemental amount of substance with values fully traceable to the SI. The method has been used by several laboratories worldwide in a number of CCQM key comparisons - interlaboratory comparison tests at the highest metrological level - supplying results equivalent to values from other methods for elemental or isotopic analysis in complex samples without the need to perform chemical destruction and dissolution of these samples. The CCOM accepted therefore in April 2007 the claim that neutron activation analysis should have the similar status as the methods originally listed by the CCOM as `primary methods of measurement`. Analytical characteristics and scope of application are given.

Optimization and validation of a LIBS method for the determination of macro and micronutrients in sugar cane leaves

Laser induced breakdown spectrometry (LIBS) was applied for the determination of macro (P, K, Ca, Mg) and micronutrients (B, Cu, Fe, Mn and Zn) in sugar cane leaves, which is one of the most economically important crops in Brazil. Operational conditions were previously optimized by a neuro-genetic approach, by using a laser Nd:YAG at 1064 nm with 110 mJ per pulse focused on a pellet surface prepared with ground plant samples. Emission intensities were measured after 2.0 mu s delay time, with 4.5 mu s integration time gate and 25 accumulated laser pulses. Measurements of LIBS spectra were based on triplicate and each replicate consisted of an average of ten spectra collected in different sites (craters) of the pellet. Quantitative determinations were carried out by using univariate calibration and chemometric methods, such as PLSR and iPLS. The calibration models were obtained by using 26 laboratory samples and the validation was carried out by using 15 test samples. For comparative purpose, these samples were also microwave-assisted digested and further analyzed by ICP OES. In general, most results obtained by LIBS did not differ significantly from ICP OES data by applying a t-test at 95% confidence level. Both LIBS multivariate and univariate calibration methods produced similar results, except for Fe where better results were achieved by the multivariate approach. Repeatability precision varied from 0.7 to 15% and 1.3 to 20% from measurements obtained by multivariate and univariate calibration, respectively. It is demonstrated that LIBS is a powerful tool for analysis of pellets of plant materials for determination of macro and micronutrients by choosing calibration and validation samples with similar matrix composition.

Gravitational quasinormal modes of AdS black branes in d spacetime dimensions

The AdS/CFT duality has established a mapping between quantities in the bulk AdS black-hole physics and observables in a boundary finite-temperature field theory. Such a relationship appears to be valid for an arbitrary number of spacetime dimensions, extrapolating the original formulations of Maldacena`s correspondence. In the same sense properties like the hydrodynamic behavior of AdS black-hole fluctuations have been proved to be universal. We investigate in this work the complete quasinormal spectra of gravitational perturbations of d-dimensional plane-symmetric AdS black holes (black branes). Holographically the frequencies of the quasinormal modes correspond to the poles of two-point correlation functions of the field-theory stress-energy tensor. The important issue of the correct boundary condition to be imposed on the gauge-invariant perturbation fields at the AdS boundary is studied and elucidated in a fully d-dimensional context. We obtain the dispersion relations of the first few modes in the low-, intermediate- and high-wavenumber regimes. The sound-wave (shear-mode) behavior of scalar (vector)-type low- frequency quasinormal mode is analytically and numerically confirmed. These results are found employing both a power series method and a direct numerical integration scheme.

Efficient method for obtaining Lep(ob)/Lep(ob)-derived animal models using adipose tissue transplantations

Background: Leptin-deficient mice (Lep(ob)/Lep(ob), also known as ob/ob) are of great importance for studies of obesity, diabetes and other correlated pathologies. Thus, generation of animals carrying the Lep(ob) gene mutation as well as additional genomic modifications has been used to associate genes with metabolic diseases. However, the infertility of Lep(ob)/Lep(ob) mice impairs this kind of breeding experiment. Objective: To propose a new method for production of Lep(ob)/Lep(ob) animals and Lep(ob)/Lep(ob)-derived animal models by restoring the fertility of Lep(ob)/Lep(ob) mice in a stable way through white adipose tissue transplantations. Methods: For this purpose, 1 g of peri-gonadal adipose tissue from lean donors was used in subcutaneous transplantations of Lep(ob)/Lep(ob) animals and a crossing strategy was established to generate Lep(ob)/Lep(ob)-derived mice. Results: The presented method reduced by four times the number of animals used to generate double transgenic models (from about 20 to 5 animals per double mutant produced) and minimized the number of genotyping steps (from 3 to 1 genotyping step, reducing the number of Lep gene genotyping assays from 83 to 6). Conclusion: The application of the adipose transplantation technique drastically improves both the production of Lep(ob)/Lep(ob) animals and the generation of Lep(ob)/Lep(ob)-derived animal models. International Journal of Obesity (2009) 33, 938-944; doi: 10.1038/ijo.2009.95; published online 16 June 2009

Neuromuscular activity during bench press exercise performed with and without the preexhaustion method

Brennecke, A, Guimaraees, TM, Leone, R, Cadarci, M, Mochizuki, L, Simao, R, Amadio, AC, and Serrao, J. Neuromuscular activity during bench press exercise performed with and without the preexhaustion method. J Strength Cond Res 23(7): 1933-1940, 2009-The purpose of the present study was to investigate the effects of exercise order on the tonic and phasic characteristics of upper-body muscle activity during bench press exercise in trained subjects. The preexhaustion method involves working a muscle or a muscle group combining a single-joint exercise immediately followed by a multi-joint exercise (e. g., flying exercise followed by bench press exercise). Twelve subjects performed 1 set of bench press exercises with and without the preexhaustion method following 2 protocols (P1-flying before bench press; P2-bench press). Both exercises were performed at a load of 10 repetition maximum (10RM). Electromyography (EMG) sampled at 1 kHz was recorded from the pectoralis major (PM), anterior deltoid (DA), and triceps brachii (TB). Kinematic data (60 Hz) were synchronized to define upward and downward phases of exercise. No significant (p > 0.05) changes were seen in tonic control of PM and DA muscles between P1 and P2. However, TB tonic aspect of neurophysiologic behavior of motor units was significantly higher (p < 0.05) during P1. Moreover, phasic control of PM, DA, and TB muscles were not affected (p > 0.05). The kinematic pattern of movement changed as a result of muscular weakness in P1. Angular velocity of the right shoulder performed during the upward phase of the bench press exercise was significantly slower (p < 0.05) during P1. Our results suggest that the strategies set by the central nervous system to provide the performance required by the exercise are held constant throughout the exercise, but the tonic aspects of the central drive are increased so as to adapt to the progressive occurrence of the neuromuscular fatigue. Changes in tonic control as a result of the muscular weakness and fatigue can cause changes in movement techniques. These changes may be related to limited ability to control mechanical loads and mechanical energy transmission to joints and passive structures.

Non-exhaustive tests for critical power estimation

Objective. - The aim of this study was to propose a new method that allows for the estimation of critical power (CP) from non-exhaustive tests using ratings of perceived exertion (RPE). Methods. - Twenty-two subjects underwent two practice trials for ergometer and Borg 15-point scale familiarization, and adaptation to severe exhaustive exercise. After then, four exercise bouts were performed on different days for the estimation of CP and anaerobic work capacity (AWC) by linear work-time equation, and CP(15), CP(17), AWC(15) and AWC(17) were estimated using the work and time to attainment of RPE15 and RPE17 based on the Borg 15-point scale. Results. - The CP, CP(15) and CP(17) (170-177W) were not significantly different (P>0.05). However, AWC, AWC(15) and AWC(17) were all different from each other. The correlations between CP(15) and CP(17), with CP were strong (R=0.871 and 0.911, respectively), but the AWC(15) and AWC(17) were not significantly correlated with AWC. Conclusion. - Sub-maximal. RPE responses can be used for the estimation of CP from non-exhaustive exercise protocols. (C) 2009 Elsevier Masson SAS. All rights reserved.

An investigation of phosphate adsorption from aqueous solution onto hydrous niobium oxide prepared by co-precipitation method

The synthetic hydrous niobium oxide has been used for phosphate removal from the aqueous solutions. The kinetic data correspond very well to the pseudo second-order equation The phosphate removal tended. to increase with a decrease of pH. The equilibrium data describe very well the Langmuir isotherm. The peak appearing at 1050 cm(-1) in IR spectra after adsorption was attributed to the bending vibration of adsorbed phosphate. The adsorption capacities are high, and increased with increasing temperature. The evaluated Delta G degrees and Delta H degrees indicate the spontaneous and endothermic nature of the reactions. The adsorptions occur with increase in entropy (Delta S positive) value suggest increase in randomness at the solid-liquid interface during the adsorption. A phosphate desorbability of approximately 60% was observed with water at pH 12, which indicated a relatively strong bonding between the adsorbed phosphate and the sorptive sites on the surface of the adsorbent. (C) 2008 Elsevier B.V. All rights reserved.

Optimization of the AZO dyes decoloration process through neural networks: Determination of the H2O2 addition critical point

The concentration of hydrogen peroxide is an important parameter in the azo dyes decoloration process through the utilization of advanced oxidizing processes, particularly by oxidizing via UV/H2O2. It is pointed out that, from a specific concentration, the hydrogen peroxide works as a hydroxyl radical self-consumer and thus a decrease of the system`s oxidizing power happens. The determination of the process critical point (maximum amount of hydrogen peroxide to be added) was performed through a ""thorough mapping"" or discretization of the target region, founded on the maximization of an objective function objective (constant of reaction kinetics of pseudo-first order). The discretization of the operational region occurred through a feedforward backpropagation neural model. The neural model obtained presented remarkable coefficient of correlation between real and predicted values for the absorbance variable, above 0.98. In the present work, the neural model had, as phenomenological basis the Acid Brown 75 dye decoloration process. The hydrogen peroxide addition critical point, represented by a value of mass relation (F) between the hydrogen peroxide mass and the dye mass, was established in the interval 50 < F < 60. (C) 2007 Elsevier B.V. All rights reserved.