899 resultados para range analysis


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A column switching LC method is presented for the analysis of fluoxetine (FLU) and norfluoxetine (NFLU) by direct injection of human plasma using a lab-made restricted access media (RAM) column. A RAM-BSA-octadecyl silica (C-18) column (40 min x 4.6 mm, 10 mu m) is evaluated in both backflush and foreflush elution modes and coupled with a C-18 lab-made (50 mm x 4.6 mm, 3 pm) analytical column in order to perform online sample preparation. Direct injection of 100 mu L, of plasma samples is possible with the developed approach. In addition, reduction of sample handling is obtained when compared with traditional liquid-liquid extraction (LLE) and SPE. The total analysis time is around 20 min. A LOQ of 15 ng/mL is achieved in a concentration range of 15-500 ng/mL, allowing the therapeutic drug monitoring of clinical samples. The precision values achieved are lower than 15% for all the evaluated points with adequate recovery and accuracy. Furthermore, no matrix interferences are found in the analysis and the proposed method shows to be an adequate alternative for analysis of FLU in plasma.

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The influence of the sample matrix in the CC-electron-capture detection analysis of the pesticides dimethoate, diazinon, chlorothalonil.. parathion methyl and fenitrothion in fruits samples has been studied. Experiments have been carried out where the pesticide responses in standard solutions prepared in selected solvent were compared with their response when present in apple, mango, papaya, banana, pineapple and melon extracts. The presence of matrix effects (MEs) and their extent were shown to be simultaneously influenced by several factors (matrix concentration, matrix type, pesticide concentration, analytical range). Pronounced MEs were observed particularly for dimethoate and diazinon in all matrices tested; in lower concentrations, all pesticides presented significant ME. The other pesticides presented variable ME. Higher ME enhancement was detected at lower pesticide concentration levels of and/or at higher matrix concentration solutions. The ME detected for fenitrothion, in the analytical range evaluated, were dependent on matrix type. For each pesticide, solvent and matrix-matched calibrations were compared for all fruit samples, and it could be concluded that quantitation based on standard solutions prepared in blank matrix extract (matrix-matched calibration) should be used to compensate the MEs and to obtain more accurate results for the pesticides studied.

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A new polymeric coating consisting of a dual-phase, polydimethylsiloxane (PDMS) and polypyrrole (PPY) was developed for the stir bar sorptive extraction (SBSE) of antidepressants (mirtazapine, citalopram, paroxetine, duloxetine, fluoxetine and sertraline) from plasma samples, followed by liquid chromatography analysis (SBSE/LC-UV). The extractions were based on both adsorption (PPY) and sorption (PDMS) mechanisms. SBSE variables, such as extraction time, temperature, pH of the matrix, and desorption time were optimized, in order to achieve suitable analytical sensitivity in a short time period. The PDMS/PPY coated stir bar showed high extraction efficiency (sensitivity and selectivity) toward the target analytes. The quantification limits (LOQ) of the SBSE/LC-UV method ranged from 20 ng mL(-1) to 50 ng mL(-1), and the linear range was from LOQ to 500 ng mL(-1), with a determination coefficient higher than 0.99. The inter-day precision of the SBSE/LC-UV method presented a variation coefficient lower than 15%. The efficiency of the SBSE/LC-UV method was proved by analysis of plasma samples from elderly depressed patients. (C) 2008 Elsevier B.V. All rights reserved.

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In a northern European climate a typical solar combisystem for a single family house normally saves between 10 and 30 % of the auxiliary energy needed for space heating and domestic water heating. It is considered uneconomical to dimension systems for higher energy savings. Overheating problems may also occur. One way of avoiding these problems is to use a collector that is designed so that it has a low optical efficiency in summer, when the solar elevation is high and the load is small, and a high optical efficiency in early spring and late fall when the solar elevation is low and the load is large.The study investigates the possibilities to design the system and, in particular, the collector optics, in order to match the system performance with the yearly variations of the heating load and the solar irradiation. It seems possible to design practically viable load adapted collectors, and to use them for whole roofs ( 40 m2) without causing more overheating stress on the system than with a standard 10 m2 system. The load adapted collectors collect roughly as much energy per unit area as flat plate collectors, but they may be produced at a lower cost due to lower material costs. There is an additional potential for a cost reduction since it is possible to design the load adapted collector for low stagnation temperatures making it possible to use less expensive materials. One and the same collector design is suitable for a wide range of system sizes and roof inclinations. The report contains descriptions of optimized collector designs, properties of realistic collectors, and results of calculations of system output, stagnation performance and cost performance. Appropriate computer tools for optical analysis, optimization of collectors in systems and a very fast simulation model have been developed.

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OBJECTIVE: This study aimed to assess women´s acceptability of diagnosis and treatment of incomplete abortion with misoprostol by midwives, compared with physicians. METHODS: This was an analysis of secondary outcomes from a multi-centre randomized controlled equivalence trial at district level in Uganda. Women with first trimester incomplete abortion were randomly allocated to clinical assessment and treatment with misoprostol by a physician or a midwife. The randomisation (1:1) was done in blocks of 12 and stratified for health care facility. Acceptability was measured in expectations and satisfaction at a follow up visit 14-28 days following treatment. Analysis of women's overall acceptability was done using a generalized linear mixed-effects model with an equivalence range of -4% to 4%. The study was not masked. The trial is registered at ClinicalTrials.org, NCT 01844024. RESULTS: From April 2013 to June 2014, 1108 women were assessed for eligibility of which 1010 were randomized (506 to midwife and 504 to physician). 953 women were successfully followed up and included in the acceptability analysis. 95% (904) of the participants found the treatment satisfactory and overall acceptability was found to be equivalent between the two study groups. Treatment failure, not feeling calm and safe following treatment, experiencing severe abdominal pain or heavy bleeding following treatment, were significantly associated with non-satisfaction. No serious adverse events were recorded. CONCLUSIONS: Treatment of incomplete abortion with misoprostol by midwives and physician was highly, and equally, acceptable to women. TRIAL REGISTRATION: ClinicalTrials.gov NCT01844024.

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The range of the Gray Wolf (Canis lupus), once covering most of North America, has been drastically reduced by an estimated 95% due to habitat loss and extermination by humans. The wolf was extirpated from Maine in the 1800’s. Wolf reintroductions have been suggested for Maine, but there is some debate about how much land is suitable for wolves. I developed a wolf habitat suitability analysis using ArcGIS and data from the Maine Office of GIS and the United States National Atlas. The model incorporates land cover, presence of major roads and railways, conservation land, industrial, non-industrial, and public woodlot ownership, distance from major points of population, deer population, and slope. The model results show areas of high and low wolf suitability in Maine. The model suggests that the best potential habitat for wolves in Maine is situated in the northwest of the state. Possible future reintroductions or natural colonization from other areas would have the highest likelihood of survival in these areas.

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We estimate optimal target-ranges of capital structure controlling for a series of firmspecific characteristics and accounting for the serial correlation that arises from the dynamic component of the leverage choice. Then, we empirically examine if firms adjust their leverages toward the estimated optimal ranges. Our analysis suggests that the observed behavior of firms is consistent with the notion of range-adjustment.

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The aim of this paper is to analyze extremal events using Generalized Pareto Distributions (GPD), considering explicitly the uncertainty about the threshold. Current practice empirically determines this quantity and proceeds by estimating the GPD parameters based on data beyond it, discarding all the information available be10w the threshold. We introduce a mixture model that combines a parametric form for the center and a GPD for the tail of the distributions and uses all observations for inference about the unknown parameters from both distributions, the threshold inc1uded. Prior distribution for the parameters are indirectly obtained through experts quantiles elicitation. Posterior inference is available through Markov Chain Monte Carlo (MCMC) methods. Simulations are carried out in order to analyze the performance of our proposed mode1 under a wide range of scenarios. Those scenarios approximate realistic situations found in the literature. We also apply the proposed model to a real dataset, Nasdaq 100, an index of the financiai market that presents many extreme events. Important issues such as predictive analysis and model selection are considered along with possible modeling extensions.

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With the increasing importance of digital communication and its distinct characteristics, marketing tools and strategies adopted by companies have changed dramatically. Among the many digital marketing tools and new media channels available for marketers, the phenomenon known as social media is one of the most complex and enigmatic. It has a range that still is quite unexplored and deeply transforms the present view on the promotion mix (Mangold & Faulds, 2009). Conversations among users on social media directly affect their perceptions on products, services and brands. But more than that, a wide range of other subjects can also become topics of conversations on social media. Hit songs, sporting events, celebrity news and even natural disasters and politics are topics that often become viral on the web. Thus, companies must grasp that, and in order to become more interesting and relevant, they must take part in these conversations inserting their brands in these online dynamic dialogues. This paper focuses on how these social interactions are manifested in the web in to two distinct cultures, Brazil and China. By understanding the similarities and differences of these cultures, this study helps firms to better adjust its marketing efforts across regions, targeting and positioning themselves, not only geographically and culturally, but also across different web platforms (Facebook and RenRen). By examining how companies should focus their efforts according to each segment in social media, firms can also maximize its results in communication and mitigate risks. The findings suggest that differences in cultural dimensions in these two countries directly affect their virtual social networking behavior in many dimensions (Identity, Presence, Relationships, Reputation, Groups, Conversations and Sharing). Accordingly, marketing efforts must be tailored to each comportment and expectations.

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Nota: A autora agradece à Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) pela concessão de bolsa de estudos para o desenvolvimento deste projeto de pesquisa.

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This paper reports on the development and optimization of a modified Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) based extraction technique coupled with a clean-up dispersive-solid phase extraction (dSPE) as a new, reliable and powerful strategy to enhance the extraction efficiency of free low molecular-weight polyphenols in selected species of dietary vegetables. The process involves two simple steps. First, the homogenized samples are extracted and partitioned using an organic solvent and salt solution. Then, the supernatant is further extracted and cleaned using a dSPE technique. Final clear extracts of vegetables were concentrated under vacuum to near dryness and taken up into initial mobile phase (0.1% formic acid and 20% methanol). The separation and quantification of free low molecular weight polyphenols from the vegetable extracts was achieved by ultrahigh pressure liquid chromatography (UHPLC) equipped with a phodiode array (PDA) detection system and a Trifunctional High Strength Silica capillary analytical column (HSS T3), specially designed for polar compounds. The performance of the method was assessed by studying the selectivity, linear dynamic range, the limit of detection (LOD) and limit of quantification (LOQ), precision, trueness, and matrix effects. The validation parameters of the method showed satisfactory figures of merit. Good linearity (View the MathML sourceRvalues2>0.954; (+)-catechin in carrot samples) was achieved at the studied concentration range. Reproducibility was better than 3%. Consistent recoveries of polyphenols ranging from 78.4 to 99.9% were observed when all target vegetable samples were spiked at two concentration levels, with relative standard deviations (RSDs, n = 5) lower than 2.9%. The LODs and the LOQs ranged from 0.005 μg mL−1 (trans-resveratrol, carrot) to 0.62 μg mL−1 (syringic acid, garlic) and from 0.016 μg mL−1 (trans-resveratrol, carrot) to 0.87 μg mL−1 ((+)-catechin, carrot) depending on the compound. The method was applied for studying the occurrence of free low molecular weight polyphenols in eight selected dietary vegetables (broccoli, tomato, carrot, garlic, onion, red pepper, green pepper and beetroot), providing a valuable and promising tool for food quality evaluation.

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Documenting the presence and abundance of the neotropical mammals is the first step for understanding their population ecology, behavior and genetic dynamics in designing conservation plans. The combination of field research with molecular genetics techniques are new tools that provide valuable biological information avoiding the disturbance in the ecosystems, trying to minimize the human impact in the process to gather biological information. The objective of this paper is to review the available non invasive sampling techniques that have been used in Neotropical mammal studies to apply to determine the presence and abundance, population structure, sex ratio, taxonomic diagnostic using mitochondrial markers, and assessing genetic variability using nuclear markers. There are a wide range of non invasive sampling techniques used to determine the species identification that inhabit an area such as searching for tracks, feces, and carcasses. Other useful equipment is the camera traps that can generate an image bank that can be valuable to assess species presence and abundance by morphology. With recent advances in molecular biology, it is now possible to use the trace amounts of DNA in feces and amplify it to analyze the species diversity in an area, and the genetic variability at intraspecific level. This is particularly helpful in cases of sympatric and cryptic species in which morphology failed to diagnose the taxonomic status of several species of brocket deer of the genus Mazama.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Propolis obtained from honeybee hives has been widely used in medicine, cosmetics, and industry due to its versatile biological activities (antioxidant, antimicrobial, fungicidal, antiviral, antiulcer, immunostimulating, and cytostatic). These activities are mainly attributed to the presence of flavonoids in propolis, which points out the interest in quantifying these constituents in propolis preparations, as well as validation of analytical methodologies. High-performance liquid chromatography (HPLC) methods have been reported to quantify isolated flavonoids or these compounds in complex biological matrices, such as herbal raw materials and extractive preparations. An efficient, precise, and reliable method was developed for quantification of propolis extractive solution using HPLC with UV detection. The chromatograms were obtained from various gradient elution systems (GES) tested in order to establish the ideal conditions for the analysis of propolis extractive solution, using methanol and water: acetonitrile (97.5 : 2.5, v/v) as mobile phase. Gradient reversed phase chromatography was performed using a stainless steel column (250 x 4.6 mm i.d., 5 mum) filled with Chromsep RP 18 (Varian), column temperature at 30.0 +/- 0.1degreesC and detection at 310 nm. The main validation parameters of the method were also determined. The method showed linearity for chrysin in the range 0.24-2.4 mug mL(-1) with good correlation coefficients (0.9975). Precision and accuracy were determined. The obtained results demonstrate the efficiency of the proposed method. The analytical procedure is reliable and offers advantages in terms of speed and cost of reagents.