Avaliação de um método de cromatografia em fase gasosa head space e estudo da estabilidade do etanol em amostras de sangue

The ethanol is the most overused psychoactive drug over the world; this fact makes it one of the main substances required in toxicological exams nowadays. The development of an analytical method, adaptation or implementation of a method known, involves a process of validation that estimates its efficiency in the laboratory routine and credibility of the method. The stability is defined as the ability of the sample of material to keep the initial value of a quantitative measure for a defined period within specific limits when stored under defined conditions. This study aimed to evaluate the method of Gas chromatography and study the stability of ethanol in blood samples, considering the variables time and temperature of storage, and the presence of preservative and, with that check if the conditions of conservation and storage used in this study maintain the quality of the sample and preserve the originally amount of analyte present. Blood samples were collected from 10 volunteers to evaluate the method and to study the stability of ethanol. For the evaluation of the method, part of the samples was added to known concentrations of ethanol. In the study of stability, the other side of the pool of blood was placed in two containers: one containing the preservative sodium fluoride 1% and the anticoagulant heparin and the other only heparin, was added ethanol at a concentration of 0.6 g/L, fractionated in two bottles, one being stored at 4ºC (refrigerator) and another at -20ºC (freezer), the tests were performed on the same day (time zero) and after 1, 3, 7, 14, 30 and 60 days of storage. The assessment found the difference in results during storage in relation to time zero. It used the technique of headspace associated with gas chromatography with the FID and capillary column with stationary phase of polyethylene. The best analysis of chromatographic conditions were: temperature of 50ºC (column), 150ºC (jet) and 250ºC (detector), with retention time for ethanol from 9.107 ± 0.026 and the tercbutanol (internal standard) of 8.170 ± 0.081 minutes, the ethanol being separated properly from acetaldehyde, acetone, methanol and 2-propanol, which are potential interfering in the determination of ethanol. The technique showed linearity in the concentration range of 0.01 and 3.2 g/L (0.8051 x + y = 0.6196; r2 = 0.999). The calibration curve showed the following equation of the line: y = x 0.7542 + 0.6545, with a linear correlation coefficient equal to 0.996. The average recovery was 100.2%, the coefficients of variation of accuracy and inter intra test showed values of up to 7.3%, the limit of detection and quantification was 0.01 g/L and showed coefficient of variation within the allowed. The analytical method evaluated in this study proved to be fast, efficient and practical, given the objective of this work satisfactorily. The study of stability has less than 20% difference in the response obtained under the conditions of storage and stipulated period, compared with the response obtained at time zero and at the significance level of 5%, no statistical difference in the concentration of ethanol was observed between analysis. The results reinforce the reliability of the method of gas chromatography and blood samples in search of ethanol, either in the toxicological, forensic, social or clinic

Desenvolvimento e validação de método analítico para determinação de teor de ácido gálico e catequina no fitoterápico sanativo® por cromatografia líquida de alta eficiência

The herbal medicine Sanativo® is produced by the Pernambucano Laboratory since 1888 with indications of healing and hemostasis. It is composed of a fluid extract about Piptadenia colubrina, Schinus terebinthifolius, Cereus peruvianus and Physalis angulata. Among the plants in their composition, S. terebinthifolius and P. colubrina have in common phenolic compounds which are assigned most of its pharmacological effects. The tannins, gallic acid and catechin were selected as markers for quality control. The aim of this study was the development and validation of analytical method by HPLC/UV/DAD for the separation and simultaneous quantification of gallic acid (GAC) and catechin (CTQ) in Sanativo®. The chromatographic system was to stationary phase, C-18 RP column, 4,6 x 150 mm (5 mm) under a temperature of 35 ° C, detection at 270 and 210 nm. The mobile phase consisted of 0.05% trifluoroacetic acid and methanol in the proportions 88:12 (v/v), a flow rate of 1 ml/min. The analytical method presented a retention factor of 0.30 and 1.36, tail factor of 1.8 and 1.63 for gallic acid and catechin, respectively, resolution of 18.2, and theoretical plates above 2000. The method validation parameters met the requirements of Resolution n º 899 of May 29, 2003, ANVISA. The correlation coefficient of linear regression analysis for GAC and CTQ from the standard solution was 0.9958 and 0.9973 and when performed from the Sanativo® 0.9973 and 0.9936, the matrix does not interfere in the range 70 to 110 %. The limits of detection and quantification for GAC and CQT were 3.25 and 0.863, and 9.57 and 2.55 mg/mL, respectively. The markers, GAC and CQT, showed repetibility (coefficient of variation of 0.94 % and 2.36 %) and satisfactory recovery (100.02 ± 1.11 % and 101.32 ± 1.36 %). The method has been characterized selective and robust quantification of GAC and CTQ in the Sanativo® and was considered validated

Desenvolvimento e validação de método analítico para determinação de WE010, WE014 e WE017

The synthetic guanylhydrazones WE010 (3,5-di-tert-butil-4-hidroxibenzaldehyde-guanylhydrazone), WE014 (4-bifenilcarboxialdehydeguanylhydrazone) and WE017 (3,4-diclorobenzaldehydeguanylhydrazone) showed high cytotoxic activity in terms of percentage inhibition of cancer cells growth. However, further progress in the development of these drug candidates requires precise and convenient methods for their qualitative and quantitative analyses. The aim of this study was to develop and validate High Performance Liquid Chromatography with diode-array detection (HPLC-DAD) and Ultra Fast Liquid Chromatography with diode-array detection (UFLC-DAD) methods suitable for as simultaneous as isolated determination of studied guanylhydrazones, based on the optimization of chromatographic parameters and obtaining reduced detection times. The chromatographic analyses of analytes by HPLC were performed on C18 ACE analytical column (150 mm x 4.6 mm), with a particle size of 5.0 μm. Among all the conditions assayed, the best results of separation were obtained with a mixture of methanol:water (60:40, v/v) as the mobile phase at a flow rate 1.5mL/min and pH of 3.5 adjusted at acetic acid. The UFLC method was developed by experimetal desing techniques in order to find optimal chromatographic analytical conditions, which were achieved on XR-ODS analytical column (50 mm x 3.0 mm), with a particle size of 2,2 μm, maintained at 25 ºC. The mobile phase was consisted of methanol:water (65:35, v/v) with 0.1% triethylamine (TEA) and pH of 3.5 adjusted at acetic acid, at a flow rate 0.5 mL/min. The procedure were validated following evaluating parameters such as specificity, linearity, limits of detection (LD) and quantification (LQ), precision, accuracy and robustness, giving results within the acceptable range. Although the UFLC method shows better sensitivity (lower values of LD and LQ), robustness (lower rates of relative standard deviation) and minimize spending time and solvent, both developed methods were adequately applied to the analysis of guanylhydrazones molecules, may be used in routine of quality control laboratories. Keywords: guanylhydrazones, HPLC/DAD, UFLC/DAD, validation of analitical method

Estimativas de mortalidade para a região nordeste do Brasil em 2010: uma associação do método demográfico equação geral de balanceamento, com o estimador bayesiano empírico

One of the greatest challenges of demography, nowadays, is to obtain estimates of mortality, in a consistent manner, mainly in small areas. The lack of this information, hinders public health actions and leads to impairment of quality of classification of deaths, generating concern on the part of demographers and epidemiologists in obtaining reliable statistics of mortality in the country. In this context, the objective of this work is to obtain estimates of deaths adjustment factors for correction of adult mortality, by States, meso-regions and age groups in the northeastern region, in 2010. The proposal is based on two lines of observation: a demographic one and a statistical one, considering also two areas of coverage in the States of the Northeast region, the meso-regions, as larger areas and counties, as small areas. The methodological principle is to use the General Equation and Balancing demographic method or General Growth Balance to correct the observed deaths, in larger areas (meso-regions) of the states, since they are less prone to breakage of methodological assumptions. In the sequence, it will be applied the statistical empirical Bayesian estimator method, considering as sum of deaths in the meso-regions, the death value corrected by the demographic method, and as reference of observation of smaller area, the observed deaths in small areas (counties). As results of this combination, a smoothing effect on the degree of coverage of deaths is obtained, due to the association with the empirical Bayesian Estimator, and the possibility of evaluating the degree of coverage of deaths by age groups at counties, meso-regions and states levels, with the advantage of estimete adjustment factors, according to the desired level of aggregation. The results grouped by State, point to a significant improvement of the degree of coverage of deaths, according to the combination of the methods with values above 80%. Alagoas (0.88), Bahia (0.90), Ceará (0.90), Maranhão (0.84), Paraíba (0.88), Pernambuco (0.93), Piauí (0.85), Rio Grande do Norte (0.89) and Sergipe (0.92). Advances in the control of the registry information in the health system, linked to improvements in socioeconomic conditions and urbanization of the counties, in the last decade, provided a better quality of information registry of deaths in small areas

A construction como método concretizador de direitos fundamentais: aplicação na jurisdição constitucional brasileira

The way of organization of the constitutional jurisdiction implies the possibility to extend the democratization of the same one in function of the popular participation in the active legitimacy to constitutional process (procedimentalist model) e, at the same time, to assure technical viable decisions fast and to the complex problems of the constitucional law (substancialist model). The comparison with the constitutional jurisdiction of U.S.A. becomes interesting from the knowledge of the wide power to decide experience of Supreme the Court that for a methodology of construction of rights and not simply of interpretation of the Constitution, brought up to date and reconstructed throughout its historical evolution the direction of the norms of basic rights and the North American principles constitutional. Construction while constitutional hermeneutic method of substancialist matrix works with techniques as the measurement of principles, the protection of interests of minorities and the entailing of the basic rights with values politicians, what it can be brought to evidence of the Brazilian constitutional jurisdiction in order to improve the construction of basic rights that comes being carried through for the judicial ativism in control of the diffuse and abstract constitutionality. To define the limits of construction is to search, on the other hand, a dialogue with the procedimentalists thesis, aiming at the widening of the participation of the citizen in the construction of the basic rights for the constitutional process and to argue forms of the society to evaluate the pronounced decisions activist in the controls diffuse and abstract of constitutionality

O discurso ideológico no método reflets-Brésil

Cette étude vise à identifier, décrire et comprendre, le discours idéologique de la méthode Reflets-Brésil. L'étude, a été subventionnée en partie par une analyze des recommandations brésiliennes, et européennes, sur l'enseignement des langues étrangères, et pour la reflexion sur le matériel d'enseignement des langues étrangères, proposées respectivement par Alain Choppin et Christian Puren, et d'autre part, trouvé appui théorique, de la proposition de John B. Thompson en ce qui concerne les concepts de la culture et l'idéologie. La recherche a été de nature qualitative, sur la base des idées de Norman Fairclough sur l'analyse critique du discours, et a été organisé autour de l'hypothèse que la méthode Reflets-Brésil, tandis que un produit de la industrie europeane du livre, adaptée pour le public brésilien, traduit le discours idéologique, malgré les recommandations brésilien en matière d'éducation et le développement des manuels scolaires. Dans l'étude, il a été conclu par la véracité de l'hypothèse. La méthode Méthode Reflets-Brésil, non seulement peut être comprise comme un véhicule idéologique, mais ne prévoit pas dans sa proposition pour l'enseignement des langues étrangères, un espace de réflexion qui peuvent conduire à une reconstruction de discours critique et / ou pratiques liées à l'enseignement du français comme langue étrangère

Análise de estruturas de superfície delgadas axissimétricas via método dos elementos finitos com utilização de elemento retilíneo

The present work deals with the linear analysis of bi-dimensional axisymmetric structures, through development and implementation of a Finite Element Method code. The structures are initially studied alone and afterwards compatibilized into coupled structures, that is, assemblages, including tanks and pressure vessels. Examples are analysed and, in order to prove accuracy, the results were compared with those furnished by the analytical solutions

Análise não-linear de treliças pelo método dos elementos finitos posicional

This work presents the positional nonlinear geometric formulation for trusses using different strain measures. The positional formulation presents an alternative approach for nonlinear problems. This formulation considers nodal positions as variables of the nonlinear system instead of displacements (widely found in literature). The work also describes the arc-length method used for tracing equilibrium paths with snap-through and snap-back. Numerical applications for trusses already established in the literature and comparisons with other studies are provided to prove the accuracy of the proposed formulation

Análise dos indicadores de qualidade versus taxa de abandono utilizando método de regressão múltipla para serviço de banda larga

Telecommunication is one of the most dynamic and strategic areas in the world. Many technological innovations has modified the way information is exchanged. Information and knowledge are now shared in networks. Broadband Internet is the new way of sharing contents and information. This dissertation deals with performance indicators related to maintenance services of telecommunications networks and uses models of multivariate regression to estimate churn, which is the loss of customers to other companies. In a competitive environment, telecommunications companies have devised strategies to minimize the loss of customers. Loosing customers presents a higher cost than obtaining new ones. Corporations have plenty of data stored in a diversity of databases. Usually the data are not explored properly. This work uses the Knowledge Discovery in Databases (KDD) to establish rules and new models to explain how churn, as a dependent variable, are related to a diversity of service indicators, such as time to deploy the service (in hours), time to repair (in hours), and so on. Extraction of meaningful knowledge is, in many cases, a challenge. Models were tested and statistically analyzed. The work also shows results that allows the analysis and identification of which quality services indicators influence the churn. Actions are also proposed to solve, at least in part, this problem

Método de avaliação do gerenciamento de resíduos em canteiro de obras da construção civil : proposta baseada em empresas construtoras da cidade de Natal-RN

According to great concern between the developed industrial activities and resultant impacts over the environment, an association of several factors have occurred, procedures to the efficient management of the rotation between economical development and the environment have been improved. A research in field have been realized inside building sites of companies in order to provide knowledge about the implemented and accomplish actions according to the resolution from CONAMA nº307. Trough the interview among the representations of the companies and photographic survey in loco, such as, what makes the companies implement this management, reutilization and recycling, transport and disposition. The present study had as objective: analyze the insertion of the used tools to residuals management, proposing improvements, in a way that it can be easily identified during the procedures execution in the building sites of the building companies of the city of Natal/RN. To reach the goal, in the first place a revision of the pertinent literature was performed; there for, it can be seen the relation between residues management and environment sustainability, once it happens in a continued way it may prevent the waste and reduces the risk that the activities way bring to the employees, community and environment; once found the great difficult faced with regard to labors, material, equipment, project, planning, costumer s interference, furnisher. And still, it could be verified wich materials generate greater indexes of residues in the works and the main occurrences of waste and loss. However a greater transparency is needed coming from the high administration in the commitment with the continued actions, to make it so, there must be a cultural change inside the company. There for there will be a greater productivity and quality of the under taking such as costumer s satisfaction

A oficina como método de desenvolvimento de projeto do produto aplicado à atividade jangadeira de Ponta Negra Natal-RN

The jangadas (brazilian fishing rafts) are rudimentary artisanal vessels intrinsic to the Northeast of Brazil. The fishery with jangadas is highly representative in the State of Rio Grande do Norte, and source of income for many families in addition to being a strong cultural icon. Is still alive despite the difficulties, bringing the history and customs of the fishermen and their people. However, is in process of extinction due to factors such as the low profitability of the activity, tourism and urbanization. From the understanding of activity involving their context and circumstances, based on identified problems regarding the conditions of use of jangadas as the unpredictability, the risk of accidents, poor working conditions, hygiene and housing, this dissertation aims to: analyzing the design of the jangada on the beach of Ponta Negra and its relationship with the activity in relation to health, safety, productivity and environment, and from such assessments, together with the results achieved during the workshops of the project, proposing a cart to move the raft, adapted to the local fisherman activity studied. To perform analysis of jangadeira activity, we used a methodology based on ergonomic work analysis - AET (WISNER, 1987; GUÈRIN, 2001; VIDAL, 2008, SALDANHA, 2004 and Carvalho, 2005). For data collection were used observational and interaction methods as a conversational action, verbalizations, photographs and video. It is emphasized that the search for solutions appropriate to the jangadeira activity was possible through the collaboration of several people, not just an informational level and understanding during the work activity, but effectively contributing to the making decisions

Aplicação do método de análise hierárquica na tomada de decisão para adoção de computação em nuvem: um estudo de caso na federação das indústrias do RN

The progresses of the Internet and telecommunications have been changing the concepts of Information Technology IT, especially with regard to outsourcing services, where organizations seek cost-cutting and a better focus on the business. Along with the development of that outsourcing, a new model named Cloud Computing (CC) evolved. It proposes to migrate to the Internet both data processing and information storing. Among the key points of Cloud Computing are included cost-cutting, benefits, risks and the IT paradigms changes. Nonetheless, the adoption of that model brings forth some difficulties to decision-making, by IT managers, mainly with regard to which solutions may go to the cloud, and which service providers are more appropriate to the Organization s reality. The research has as its overall aim to apply the AHP Method (Analytic Hierarchic Process) to decision-making in Cloud Computing. There to, the utilized methodology was the exploratory kind and a study of case applied to a nationwide organization (Federation of Industries of RN). The data collection was performed through two structured questionnaires answered electronically by IT technicians, and the company s Board of Directors. The analysis of the data was carried out in a qualitative and comparative way, and we utilized the software to AHP method called Web-Hipre. The results we obtained found the importance of applying the AHP method in decision-making towards the adoption of Cloud Computing, mainly because on the occasion the research was carried out the studied company already showed interest and necessity in adopting CC, considering the internal problems with infrastructure and availability of information that the company faces nowadays. The organization sought to adopt CC, however, it had doubt regarding the cloud model and which service provider would better meet their real necessities. The application of the AHP, then, worked as a guiding tool to the choice of the best alternative, which points out the Hybrid Cloud as the ideal choice to start off in Cloud Computing. Considering the following aspects: the layer of Infrastructure as a Service IaaS (Processing and Storage) must stay partly on the Public Cloud and partly in the Private Cloud; the layer of Platform as a Service PaaS (Software Developing and Testing) had preference for the Private Cloud, and the layer of Software as a Service - SaaS (Emails/Applications) divided into emails to the Public Cloud and applications to the Private Cloud. The research also identified the important factors to hiring a Cloud Computing provider

Produção artesanal : análise do método de intervenção de design no artesanato potiguar sob o ponto de vista dos atores envolvidos no processo

This work presents an analysis of the method of intervention used in the craft of design by SEBRAE in Rio Grande do Norte under the viewpoint of the actors involved, especially the craftsmen and design consultants. The research methodology used was based on the ergonomic work analysis - AET, applying observational techniques and interactive. Data tabulated from the matrix to include comments were analyzed in order to allow the generation of qualitative and quantitative information. The results of this research allow us to affirm that for the process of innovation through the design of intervention are satisfactory for all involved, it is necessary that the bonds of interaction are established and the joint actions in the innovation process to bear fruit in favor sustainability of artisan groups

Uma aplicação de análise de decisão com o método AHP Processo de hierarquia analítica: um estudo sobre adoção de Sistema eletrônico de cobrança no Transporte público urbano

This thesis carries through an application of Analysis of Multicriterion Decision with use of the method of Analytical Hierarchy Process (AHP) in the problematic one of taking of decision of the adoption of electronic collecting in the system of urban transport in the country, a subject that has been controversial. A modeling of criteria and alternatives is carried through and applied a questionnaire based on method AHP the excellent actors in the system of urban transport - Leading of the Managing Agency Public Municipal theatre of Urban Transports, Controller of Company of Bus, Controller of Labor union, Controller of Union of Companies, Communitarian Leader. The considered alternatives were: the maintenance of the current state with collectors, the implementation of electronic collection without collectors, and the implementation of electronic collection with collectors. The used criteria were: job, impact in the fare, control of the system, easiness of use, information. The study was carried through in the city of Natal, RN, where if the adoption of electronic collection argues and where this implementation in some bus lines between Natal and Parnamirim exists, city that integrates the region of the great Natal. The main results of the method evidence in a dimension, the viability of use of method AHP with questionnaire by means of validation of the judgments with analysis of variance beyond proper the normal mechanisms of analysis of consistency to the method, and in another one, the contribution of the analysis boarding multicriterion to become the judgments more clearly. The main results of the analysis help to show that although to models of criteria and distinct judgments of the actors, the method evidenced that it has inclination the adoption of the electronic collection on the current situation, even so with divergences between the maintenance or not of the collector. The research points to the possibility of accomplishment of the application of the AHP in successive rounds of judgments

Um algoritmo para estimação de estado em alimentadores de distribuição de energia elétrica com base no método da soma de potências

Most algorithms for state estimation based on the classical model are just adequate for use in transmission networks. Few algorithms were developed specifically for distribution systems, probably because of the little amount of data available in real time. Most overhead feeders possess just current and voltage measurements at the middle voltage bus-bar at the substation. In this way, classical algorithms are of difficult implementation, even considering off-line acquired data as pseudo-measurements. However, the necessity of automating the operation of distribution networks, mainly in regard to the selectivity of protection systems, as well to implement possibilities of load transfer maneuvers, is changing the network planning policy. In this way, some equipments incorporating telemetry and command modules have been installed in order to improve operational features, and so increasing the amount of measurement data available in real-time in the System Operation Center (SOC). This encourages the development of a state estimator model, involving real-time information and pseudo-measurements of loads, that are built from typical power factors and utilization factors (demand factors) of distribution transformers. This work reports about the development of a new state estimation method, specific for radial distribution systems. The main algorithm of the method is based on the power summation load flow. The estimation is carried out piecewise, section by section of the feeder, going from the substation to the terminal nodes. For each section, a measurement model is built, resulting in a nonlinear overdetermined equations set, whose solution is achieved by the Gaussian normal equation. The estimated variables of a section are used as pseudo-measurements for the next section. In general, a measurement set for a generic section consists of pseudo-measurements of power flows and nodal voltages obtained from the previous section or measurements in real-time, if they exist -, besides pseudomeasurements of injected powers for the power summations, whose functions are the load flow equations, assuming that the network can be represented by its single-phase equivalent. The great advantage of the algorithm is its simplicity and low computational effort. Moreover, the algorithm is very efficient, in regard to the accuracy of the estimated values. Besides the power summation state estimator, this work shows how other algorithms could be adapted to provide state estimation of middle voltage substations and networks, namely Schweppes method and an algorithm based on current proportionality, that is usually adopted for network planning tasks. Both estimators were implemented not only as alternatives for the proposed method, but also looking for getting results that give support for its validation. Once in most cases no power measurement is performed at beginning of the feeder and this is required for implementing the power summation estimations method, a new algorithm for estimating the network variables at the middle voltage bus-bar was also developed