29 resultados para CG-EM

em Universidade Federal do Rio Grande do Norte(UFRN)


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PAHs (Polycyclic Aromatic Hydrocarbons) are a group of organic substances which receive considerable attention because of the carcinogenic and mutagenic properties of some of them. It is therefore important to determine the PAHs in different environmental matrices. Several studies have shown the use of gas chromatography coupled to mass spectrometry as a technique for quantification of PAHs by presenting excellent detection limits. This study aimed to develop an analytical methodology for the determination of 16 PAHs listed by the USEPA, test two methods for extraction of PAHs in water from a 23 factorial design, quantify them through the analytical technique coupled to gas chromatography mass spectrometry (GC/MS) using the method developed, and finally apply the results in chemometrics. The sample was synthesized and subjected to tests of the 23 factorial design, which has the factors: the type of extraction technique (ultrasound and digester), the ratio solvent / sample (1:1 and 1:3) and the type of solvent (dichloromethane / hexane and acetone / dichloromethane). The responses of eight combinations of the factorial design were obtained from the quantification by external calibration in GC/MS. The quantification method was developed from an optimized adaptation of the USEPA Method 8270. We used the full scan mode as a way of acquiring the mass spectra of 16 PAHs. The time in which the samples were subjected to ultrasound was fixed at 10 min and held an investigation to establish the conditions of power and time in the digester. We had the best response in the investigation of the digester power of 100 watts and the time of six minutes. The factorial design of liquid-liquid extraction showed that the most representative factors were: the use of the digester as extraction technique, the ratio solvent / sample 1:1 and the use of a 1:1 mixture of dichloromethane / hexane as a solvent more suitable. These results showed that the 1:1 mixture of dichloromethane / hexane is an excellent mixture to recover the extraction of PAHs an aqueous sample using the microwave digester. The optimization of the method of separation, identification and quantification of PAHs in the GC/MS was valid for 16 PAHs present in each chromatogram of the samples

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Tangara da Serra is located on southwestern Mato Grosso and is found to be on the route of pollutants dispersion originated in the Legal Amazon s deforestation area. This region has also a wide area of sugarcane culture, setting this site quite exposed to atmospheric pollutants. The objective of this work was to evaluate the genotoxicity of three different concentrations of organic particulate matter which was collected from August through December / 2008 in Tangara da Serra, using micronucleus test in Tradescantia pallida (Trad-MCN). The levels of particulate matter less than 10μm (MP10) and black carbon (BC) collected on the Teflon and polycarbonate filters were determined as well. Also, the alkanes and polycyclic aromatic hydrocarbons (PAHs) were identified and quantified on the samples from the burning period by gas chromatography detector with flame ionization detection (GC-FID). The results from the analyzing of alkanes indicate an antropic influence. Among the PAHs, the retene was the one found on the higher quantity and it is an indicator of biomass burning. The compounds indene(1,2,3-cd)pyrene and benzo(k)fluoranthene were identified on the samples and are considered to be potentially mutagenic and carcinogenic. By using Trad-MCN, it was observed a significant increase on the micronucleus frequency during the burning period, and this fact can be related to the mutagenic PAHs which were found on such extracts. When the period of less burnings is analyzed and compared to the negative control group, it was noted that there was no significant difference on the micronuclei rate. On the other hand, when the higher burning period is analyzed, statistically significant differences were evident. This study showed that the Trad-MCN was sensible and efficient on evaluating the genotoxicity potencial of organic matter from biomass burning, and also, emphasizes the importance of performing a chemical composition analysis in order to achieve a complete diagnosis on environmental risk control

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The Vitamin E consists of eight chemically homologous forms, designated alpha, beta, gamma and delta tocopherols and tocotrienols. Biologically, the alpha-tocopherol (α-TOH) is the most important. Commercially, are found two types of α-TOH a natural (RRR-alpha-tocopherol) and another synthetic (all-rac-alpha-tocopherol). Both forms are absorbed in the intestine, the liver is a preference in favor of forms 2R, due to transfer protein α-TOH. It has higher affinity to these stereoisomers. Newborns are considered high risk for vitamin E deficiency, mainly premature, these have breast milk as a food source for maintenance of serum α-TOH. Clinical signs such as thrombocytosis, hemolytic anemia, retrolental fibroplasia, intraventricular hemorrhage, bronchopulmonary dysplasia and spinocerebellar degeneration can be found in case of a low intake of α-TOH. Thus, maternal supplementation on postpartum with α-TOH can be an efficient way to increase levels of vitamin E in breast milk and thus the consequently increase the supply of micronutrient for the newborn. However, most studies with vitamin E supplementation have been conducted in animals and little is known about the effect of maternal supplementation in humans, as well as on its efficiency to increase levels of α-TOH in human milk, depending on the shape natural or synthetic. The study included 109 women, divided into three groups: control without supplementation (GC) (n=36), supplemented with natural capsule (GNAT) (n=40) and the synthetic capsule (GSINT) (n=33). Blood samples were collected for determination of maternal nutritional status, and colostrums at initial contact and after 24 hours post-supplementation. Analyses were performed by High Performance Liquid Chromatography. Values of α-TOH in serum below 499.6mg/dL were considered deficient. We used the Kruskal-Wallis test and Tukey test to confirm the increase of alpha-tocopherol in milk and efficiency of administered capsules. Daily consumption of α-TOH was based on daily intake of 500 mL of colostrum by the newborn and compared with the nutritional requirement for children from 0 to 6 months of age, 4 mg / day. The mothers had mean concentration of serum α-TOH in 1016 ± 52, 1236 ± 51 and 1083 ± 61 mg / dL, in CG, GNAT and GSINT respectively. There were no women with deficiiency. The GC did not change the concentrations of α-TOH in colostrum. While women supplemented with natural and synthetic forms increased concentrations of α-TOH colostrum in 57.6% and 39%, respectively. By comparing supplemented groups, it was observed a significant difference (p=0.04), the natural capsule more efficient than the synthetic, approximately 49.6%. Individually, 21.1% of the women provided below 4mg/day of α-TOH, after supplementation for this index declined4.1%. Thus, maternal supplementation postpartum raised the levels of alpha-tocopherol in colostrum, and increased efficiency was observed with the natural form

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Estuaries are environments prone to the input of chemical pollutants of various kinds and origins, including polycyclic aromatic hydrocarbons (PAHs). Anthropogenic PAHs may have two possible sources: pyrolytic (with four or more aromatic rings and low degree of alkylation) and petrogenic (with two and three aromatic rings and high degree of alkylation). This study aimed to evaluate the levels, distribution and possible sources of polycyclic aromatic hydrocarbons in the estuary of the Potengi river, Natal, Brazil. Samples of bottom sediments were collected in the final 12 km of the estuary until its mouth to the sea, where the urbanization of the Great Natal is more concentrated. Sampling was performed on 12 cross sections, with three stations each, totaling 36 samples, identified as T1 to T36. The non alkylated and alkylated PAHs were analyzed by gas chromatography coupled to mass spectrometry (GC / MS). PAHs were detected in all 36 stations with total concentration on each varying 174-109407 ng g-1. These values are comparable to those of several estuarine regions worldwide with high anthropogenic influence, suggesting the record of diffuse contamination installed in the estuary. PAHs profiles were similar for most stations. In 32 of the 36 stations, low molecular weight PAHs (with 2 and 3 ring: naphthalene, phenanthrene and their alkylated homologues) prevailed, which ranged from 54% to 100% of the total PAH, indicating that leaks, spills and combustion fuels are the dominant source of PAH pollution in the estuary. The level of contamination by PAHs in most stations suggests that there is potential risk of occasional adverse biological effects, but in some stations adverse impacts on the biota may occur frequently. The diagnostic ratios could differentiate sources of PAHs in sediments of the estuary, which were divided into three groups: petrogenic, pyrolytic and mixing of sources. The urban concentration of the Great Natal and the various industrial activities associated with it can be blamed as potential sources of PAHs in bottom sediments of the estuary studied. The data presented highlight the need to control the causes of existing pollution in the estuary

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The retail fuel stations are partially or potentially polluters and generators of environmental accidents, potentially causing contamination of underground and surface water bodies, soil and air. Leaks in fuel retail stations´ underground storage systems are often detected in Brazil and around the world. Monoaromatic hydrocarbons, BTEX (benzene, toluene, ethylbenzene and xylenes) and polycyclic aromatic hydrocarbons (PAHs) are an indication of the presence of contamination due to its high toxicity. This paper presents a case study of contamination in a Fuel Retail Station by petroleum derivative products in the city of Natal. For identification and quantification of the hydrocarbons, EPA analytical methods were used. The values of benzene quantified by EPA method 8021b CG-PID/FID, ranged from 1.164 to 4.503 mg.Kg-1 in soil samples, and from 12.10 to 27,639 μg.L-1 in underground water samples. Among the PAHs, naphthalene and anthracene showed the most significant results in soil samples, 0.420 to 15.46 mg.Kg-1 and 0.110 to 0,970 mg.Kg-1, respectively. In underground water samples, the results for Naphthalene varied between 0.759 and 614.7 μg.L-1. PAHs were quantified by EPA Method 8270 for GCMS. All of the results for the chemical analysis were compared with the values for the CONAMA 420/2009 resolution. The results for benzene (27,639 μg.L-1) showed levels highly above the recommended by the CONAMA 420 resolution, wherein the maximum permissible for underground water is 5 μg.L-1. This is a worrying factor, since underground water makes up 70% of the city of Natal´s water supply

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior

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Changes introduced by cardiopulmonar and neuromuscular training on basal serum insulin-like grow factor-1 (IGF-1) and cortisol levels, functional autonomy and quality of life in elderly women The aim of this study was to compare the effects of strength and aerobic training on basal serum IGF-1 and Cortisol levels, functional autonomy (FA) and quality of life (QoL) in elderly women after 12 weeks of training. The subjects were submitted the strength training (75-85% 1-RM) with weight exercises (SG; n=12; age=66.08 ± 3,37 years; BMI=26,77 ± 3,72 kg/m2), aerobic training with aquatic exercises (AG; n=13; age=68,69 ± 4,70 years; BMI=29,19 ± 2,96 kg/m2) and control group (CG; n=10; age=68,80 ± 5,41 years; BMI=29,70 ± 2,82 kg/m2). Fasting blood was analyzed to measure basal IGF-1 and cortisol levels by chemiluminescence method. The t-Student test showed increased IGF-1 in the SG (p<0.05) for intragroup comparison. The Repeated-measure ANOVA presented increased IGF-1 (p<0.05) in the SG compared to the other two groups. There were no differences in cortisol levels. All the FA tests (GDLAM autonomy protocol) presented decreased significant in the time marked in seconds to the SG. The same results were found in the AG, except in the rise from a sitting position test. The autonomy index presented significant improvements (p<0.05) in the SG related to the AG and CG and in the AG to the CG. The SG showed increased QoL (p<0.05) (by WHOQOL-Old questionnaire) in the facet 1 (sensorial functioning) and facet 5 (death and dying). Thus, the SG obtained positive changes on IGF-1 and FA levels when compared to the AG. This suggests that strength training can indicated to decrease the effects of ageing.

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A resistência microbiana a antimicrobianos tem favorecido a busca por substâncias bioativas provenientes de plantas usadas na medicina popular, com o intuito de se obter novos fármacos com atividade antimicrobiana. Neste estudo, foi proposta a investigação da atividade antibacteriana do óleo-resina de Copaifera duckei e de diferentes extratos da casca de Pseudobombax marginatum, e seus possíveis mecanismos de ação. O potencial inibitório antibacteriano foi avaliado utilizando-se os métodos de difusão e diluição em ágar, e a bioautografia. O mecanismo de ação foi analisado por microscopia eletrônica, no qual se observou alterações na ultraestrutura bacteriana, e por eletroforese em SDS-PAGE, que determinou ação sobre as proteínas das superfícies celulares. A análise química foi realizada pelas técnicas de Espectrometria de massas acoplada ao Cromatógrafo a gás- EM/CG (C. duckei) e Cromatografia Líquida de Alta Eficiência- CLAE (P. marginatum). Entre as bactérias estudadas, B. cereus foi a mais suscetível às plantas em estudo, com concentrações inibitórias mínimas (CIMs) correspondentes a 0,3125 mg/mL para o óleo-resina de copaíba, e 0,5 mg/mL para extrato hidroalcoólico (1:1) e 0,512 mg/mL para a fração butanólica da casca P. marginatum, nos quais pôde-se observar alterações na parede celular do B. cereus, com remoção da camada S, espessamento da parede celular e formação de diversos septos nos centros de divisão celular. A análise química por EM/CG mostrou compostos terpênicos no óleo-resina de C. duckei, tendo como composto majoritário o β-bisaboleno, e a análise por CLAE mostrou a presença de compostos derivados da catequina na casca do P. marginatum. Desta forma, as plantas em estudo mostram um potencial antibacteriano considerável, podendo contribuir tanto na terapia antimicrobiana como na área de alimentos, tendo como um de seus prováveis sítios de ação a parede celular bacteriana

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The epilepsy is one of the neurological disorders more common in the pediatric period, and which interferes significantly in the psycho and social life of children and teenagers. The objective of this study was analyzing the practice of sedentary practices, physicals, traditional infant fun and games of children and teenagers with and without epilepsy. The study was prospective, transversal descriptive, done with 60 children and teenagers with epilepsy (Epileptic Group - EG) patients from Pediatric Neurology Clinic of the Centre Integrated Health Lineu Araújo and 60 children and teenagers without epilepsy (Control Group - CG) students from municipal public school, both of the two groups paired with the same age (age group 7 to 14 years) of both the genders (female = 25/41,6% and male = 35/58,3%) of the Teresina city Piauí. It was done two pattern questionnaires, one applied to children and teenagers of the EG and CG to identify the sedentary activities, physical and traditional infant games and other to the parents/responsible of the EG about the clinical and demographic information. The results permitted the elaboration of two manuscripts: a) the first one titled The Practice of Sedentary and Physical Activities of Children and Teenagers with Epilepsy which showed significant difference in the sedentary activities of playing with car toy (p=0,021) to the EG and reading to the CG (p=0,001); in the physical activities the school physical education (p=0,001) and riding a bike (p=0,014) to the CG; b) the second one The Practice of Infant Games and Fun the children and teenagers with and without Epilepsy in this one the playing with marble presented significant difference (p=0,016) to the CG, despite the girls of the two groups don t do this activity. Observing the distribution of frequencies, it was verified that in the play catch-up and hide-and-seek and burn the EG plays more than the CG both in female and male gender. The girls of the EG play less skip, 60 while the boys of the two groups don t play. Elastic jump the girls of the two groups play in a same frequency and the boys don t participate of this fun. The seizures were found to occur during: soccer (23,3%); hide-and-seek (6,6%) and running (3,3%). In the sedentary activities, seizures were reported to occur: resting and watching TV (18,3%), sleeping (36,0%); sitting (13,3%) and lying down (11,7%). Our results showed that the epileptic group and the controls group engage in the same activities, although the epileptic group participates less than the controls. Although the EG had presented a bigger percentage of generalized attacks, they don t occur during the practice of formal physical activities. The research was developed by a multidisciplinary team, and this contributed a lot to the realization of this study

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The extraction with pressurized fluids has become an attractive process for the extraction of essential oils, mainly due the specific characteristics of the fluids near the critical region. This work presents results of the extraction process of the essential oil of Cymbopogon winterianus J. with CO2 under high pressures. The effect of the following variables was evaluated: solvent flow rate (from 0.37 to 1.5 g CO2/min), pressure (66.7 and 75 bar) and temperature (8, 10, 15, 20 and 25 ºC) on the extraction kinetics and the total yield of the process, as well as in the solubility and composition of the C. winterianus essential oil. The experimental apparatus consisted of an extractor of fixed bed and the dynamic method was adopted for the calculation of the oil solubility. Extractions were also accomplished by conventional techniques (steam and organic solvent extraction). The determination and identification of extract composition were done by gas chromatography coupled with a mass spectrometer (GC-MS). The extract composition varied in function of the studied operational conditions and also related to the used extraction method. The main components obtained in the CO2 extraction were elemol, geraniol, citronellol and citronellal. For the steam extraction were the citronellal, citronellol and geraniol and for the organic solvent extraction were the azulene and the hexadecane. The most yield values (2.76%) and oil solubility (2.49x10-2 g oil/ g CO2) were obtained through the CO2 extraction in the operational conditions of T = 10°C, P = 66.7 bar and solvent flow rate 0.85 g CO2/min

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The decontamination of the materials has been subject of some studies. One of the factors that it increases the pollution is the lack of responsibility in the discarding of toxic trash, as for example the presence of PCB (Polychlorinated Biphenyls) in the environment. In the Brazilian regulations, the material contaminated with PCB in concentrations higher than 50 ppm must be stored in special places or destroyed, usually by incineration in plasma furnace with dual steps. Due to high cost of the procedure, new methodologies of PCBs removal has been studied. The objective of this study was to develop an experimental methodology and analytical methodology for quantification of removal of PCBs through out the processes of extractions using supercritical fluid and Soxhlet method, also technical efficiency of the two processes of extraction, in the treatment of contaminated materials with PCBs. The materials studied were soils and wood, both were simulated contamination with concentration of 6.000, 33.000 and 60.000 mg of PCB/ kg of materials. Soxhlet extractions were performed using 100 ml of hexane, and temperature of 180 ºC. Extractions by fluid supercritical were performed at conditions of 200 bar, 70°C, and supercritical CO2 flow-rate of 3 g/min for 1-3 hours. The extracts obtained were quantified using Gas chromatography-mass spectrometry (GC/MS). The conventional extractions were made according to factorial experimental planning technique 22, with aim of study the influence of two variables of process extraction for the Soxhlet method: contaminant concentration and extraction time for obtain a maximum removal of PCB in the materials. The extractions for Soxhlet method were efficient for extraction of PCBs in soil and wood in both solvent studied (hexane and ethanol). In the experimental extraction in soils, the better efficient of removal of PCBs using ethanol as solvent was 81.3% than 95% for the extraction using hexane as solvent, for equal time of extraction. The results of the extraction with wood showed statistically it that there is not difference between the extractions in both solvent studied. The supercritical fluid extraction in the conditions studied showed better efficiency in the extraction of PCBs in the wood matrix than in soil, for two hours extractions the obtain percentual of 43.9 ± 0.5 % for the total of PCBs extracted in the soils against 95.1 ± 0,5% for the total of PCBs extracted in the wood. The results demonstrated that the extractions were satisfactory for both technical studied

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This dissertation aims the development of an experimental device to determine quantitatively the content of benzene, toluene and xylenes (BTX) in the atmosphere. BTX are extremely volatile solvents, and therefore play an important role in atmospheric chemistry, being precursors in the tropospheric ozone formation. In this work a BTX new standard gas was produced in nitrogen for stagnant systems. The aim of this dissertation is to develop a new method, simple and cheaper, to quantify and monitor BTX in air using solid phase microextraction/ gas chromatography/mass spectrometry (SPME/CG/MS). The features of the calibration method proposed are presented in this dissertation. SPME sampling was carried out under non-equilibrium conditions using a Carboxen/PDMS fiber exposed for 10 min standard gas mixtures. It is observed that the main parameters that affect the extraction process are sampling time and concentration. The results of the BTX multicomponent system studied have shown a linear and a nonlinear range. In the non-linear range, it is remarkable the effect of competition by selective adsorption with the following affinity order p-xylene > toluene > benzene. This behavior represents a limitation of the method, however being in accordance with the literature. Furthermore, this behavior does not prevent the application of the technique out of the non-linear region to quantify the BTX contents in the atmosphere.

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PURPOSE: To examine the acute effects caused by three techniques for stretching the hamstrings muscle on the active concentric peak torque (PT), passive PT and electromyographic activity (EMG). METHODS: Sixty volunteers (mean ± SD age, 22.6 ± 3 years), height 1.64 ± 0.07m and body weight of 58 ± 8.6kg, were randomly allocated into 4 groups of 15 subjects: Control Group (CG) - 5 minutes at rest, Static Stretching Group (SG) - 2 x 30s; Hold-Relax Group (HRG) - 3 x 6s of isometric contraction of hamstrings interspersed by 10s of hamstrings stretching and agonist Hold-Relax Group (AHRG) - 3 x 6s of isometric contraction of the quadriceps interspersed by 10s of hamstrings stretching. Evaluation has been conducted preand post-intervention, which verified the active concentric PT, passive PT EMG activity of IT. The statistical inference was performed by testing intra and inter, significance level at 5%. RESULTS: After intervention, there was a reduction in passive PT on CG, accompanied by a reduction of EMG activity, and an increase in passive PT on SG and AHRG. There was no change in the active concentric PT, or change in EMG activity. CG showed an increase in angle of the PT active, while the other groups showed no change. CONCLUSION: The results suggest that the shortterm stretching: 1) causes acute increase in passive torque, since the muscle does not perform sub-maximal contraction, 2) does not change in electromyographic activity and active torque, ind ependent of the technique

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Physical Exercise (PE) is a necessary component in the management in COPD patients, where respiratory symptoms are associated with reduced functional capacity. Even with the increase in the number of studies that have been published and the therapeutics success using aquatic therapy approach, studies using PE in water in COPD patients are so few. Objective: the aim of this present study was to analyze the effects of low intensity water exercise in COPD patients, developed in two different places aquatic and ground. Methods: This is a randomized clinical trial study, 42 patients with moderate to very severe DPOC were recruited for the study, mean age of 63,2  10,9 years old. Randomized in 3 groups: Control Group (CG), Land Group (LG) and Water Group (WG). The PE protocol was performed in a period of 8 weeks, with frequency of 3 times per week. The CG participated in an educational program. All the patients were assessed twice through spirometry, respiratory muscular strength, the 6-min walk test, the quality of life (SF-36 and SGRQ), the LCADL, the MRC, the BODE index and the upper limbs (UP) incremental test. Results: There was a significant difference after the approaches in DP6 from the WG (p=0,02); in VEF1 in LG (p=0,00) and WG (p=0,01); in MIP in LG (p=0,01) and WG (p=0,02); in MEP in LG (p=0,02) and WG (p=0,01); the MRC decreases in WG (p=0,00). there was an increase of the weight supported by the UP in LG (p=0,00) and WG (p=0,01). The LG showed an increase of the quality of life represented by the SGRQ total score (p=0,00). The BODE index decreased in LG (p=0,00) and WG (p=0,01). In LCDAL, the LG showed a decrease. Conclusion: This data in this present study suggest that both approaches of low intensity exercise showed to be beneficial in moderate to very severe COPD patients. The WG showed additional benefits in physical function, pointing to a new therapeutic modality for COPD patients

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To analyze the effects of electrical stimulation at two frequencies on the EMG parameters (EMG) and dynamometer, in muscles with different typing. MATERIALS AND METHODS: This is a controlled clinical trial, randomized and double blind. Sixty healthy volunteers (23.6 ± 4.2anos; 54.2 ± 7.7kg, 1.62 ± 0.009 cm) of both sexes were divided randomly into three groups: control group (CG), experimental group 1 (SG1) with application of the current Russian 30 HZ and experimental group 2 (EG2) at 70 Hz The volunteers performed an initial assessment (AV1) on the isokinetic dynamometer with three repetitions maximum voluntary isometric (MVC) for knee extension concomitant uptake of EMG for the VM muscle, VL and RF. Later, after application of NMES, they underwent an experimental protocol of isometric fatigue using 70% of MVIC, ending with the completion of a final assessment (AV2) in the same manner as the AV1. RESULTS: By analyzing the profile of the 60 subjects in three broad, VM showed a higher value of RMS behavior when the VL and RF (p = 0.03 and p = 0.02). With respect to Fmed the RF muscle (p = 0.001) showed a higher value for the VM. The VM muscle showed significant increases of Fmed (p = 0.05) after electrical stimulation at 70 Hz when compared the AV1 AV2 and RF showed significant decreases (p = 0.009) after stimulation at 30 Hz during the fatigue showed an increase RMS in the VM and VL, with a reduction in RF. For the variable Fmed was observed in three broad decline during fatigue. CONCLUSION: Our findings provide evidence that the muscles VM, VL and RF fiber typing are different besides indicating that the frequency of NMES tend to relate to the muscle stimulated. Finally suggests the surface EMG as a noninvasive method for characterizing muscle