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

Alcoolemia em vítimas fatais de acidentes de trânsito no Rio Grande do Norte empregando cromatografia em fase gasosa - head space

Alcohol is one of the few psychotropic drugs that their consumption has admitted legally and sometimes encouraged by the society. Studies show alcohol as the highest consumption of drugs among young people and society in general, probably because of its availability and easy access. The abuse causes public health problems, which was closely related to the violence, socioeconomic problems and the high number of automobile accidents. Transit is one of the main sectors affected by the effects of alcohol, observing a high incidence in the studies. About half of automobile accidents occurs after the consumption of alcoholic beverage, and the vast majority of cases related to high concentrations of alcohol in the bloodstream. The relationship of drunk with traffic accidents is in fact evident everywhere in the world, including Brazil, where studies have shown a high relationship between alcohol consumption and traffic accidents. This study determined the alcohol in fatal victims of traffic accidents in the state of Rio Grande do Norte and established the profile of this population compared with those found in Brazil and other countries. Samples of blood of ethanol added to fulfillment of the standardization of chromatographic conditions and procedures for the analysis, being employed in the determination of alcohol in blood samples of 277 victims of traffic accidents, collected at the Institute of Scientific Technical Police of Rio Grande do North (ITEP) in the year 2007. The blood alcohol level was determined in these samples correlated with the sex, age and marital status of the victim and the location, day of week and month when the accident occurred, is doing a statistical analysis and outlining a profile of the victims of an accident at transit in the state of Rio Grande do Norte. The parameters of standardization studied ensured the quality of the analytical method and, consequently, to obtain reliable laboratory results. Being given the best temperature for injector (150 ºC), detector (250 ºC) and column (50 ºC) with a flow of gas in the column of 2mL/minutos and analysis of time of 12 minutes. The method was linear in the range of 0.01 to 3.2 g / L (r2 = 0.9989) with average recovery of 100.2% and precision with coefficient of variation less than 15%. The analysis carried out on victims of fatal road traffic accidents, ethanol detected in the blood in 66.43% of the victims and these, 96% showed concentration ≥ 0.2 g / L, 87.73% of victims were male, while 12.27% female. The younger age group (1535 years) was the most involved (52,35%) and most single (55.60%). The accidents occurred with greater prevalence in the day on Monday (27%) followed by Sunday (24,19%) and Saturday (15,52%) and it was found that the prevalence of injuries varied between the different months of the year, and in February (14.4%) and April (10.47%) the months that had a higher number of accidents, however this oscillation showed no statistically significant difference. Also no significant difference was observed between the tracks of concentration found in men and women. The standardized method showed to be efficient, given satisfactorily to the goals of this work, and the high levels of alcohol found in victims of fatal road traffic accidents are consistent with several studies of literature, and the profile of the victim also supported by presenting in its most young adults, male and single

Efeitos do alongamento e do aquecimento no desempenho isocinético e na atividade eletromiográfica do músculo bíceps femoral ensaio clínico randomizado

To evaluate the effects of warm-up and stretching, singly or combined, on isokinetic performance and electromyographic activity of the biceps femoris. Materials and methods: Sixty-four volunteers of both sexes, with mean age of 23,1 ± 3,5 years and mean body mass index of 23,5 ± 2,5 Kg/m2 were randomly assigned into 4 groups: control, warm-up (stationary bicycle for 10 minutes), stretching (4 sets of 30 seconds of hamstring muscles static stretching) and warm-up + stretching. All the volunteers were submitted to evaluation pre and post-intervention of the muscle latency time and biceps femoris RMS and the passive torque, peak torque and power of the hamstring muscles. Results: The warm-up + stretching group had reduction of muscle latency time. There was a reduction of RMS during passive torque evaluation in stretching group. The RMS during isometric evaluation was reduced in all experimental groups. The RMS during eccentric evaluation showed reduction in control and warm-up + stretching groups. The passive torque and the eccentric peak torque had no significant differences pre to post-intervention in any group. There was reduction in isometric peak torque in all groups. Conclusion: The warm-up and stretching, when applied in combination can reduce the muscle latency time; stretching protocol promoted neural changes; the protocols used did not alter the muscle viscoelastic properties

Influência da fadiga no comportamento neuromuscular do quadríceps femoral, após reconstrução do ligamento cruzado anterior

Muscle fatigue is a phenomenon that promotes physiological and biomechanical disorders and their changes in healthy subjects have been widely studied and have significant importance for care in preventing injuries, but we do not have many information about its effects in patients after ACL reconstruction. Thus, this study is to analyze the effects of fatigue on neuromuscular behavior of quadriceps after ACL reconstruction. To reach this objective, participants were forty men, twenty healthy (26,90 ± 6,29 years) and twenty after ACL reconstruction (29,75 ± 7,01 years) with a graft of semitendinosus and gracilis tendons, between four to six months after surgery. At first, there was an assessment of joint position sense (JPS) at the isokinetic dynamometer at a speed of 5°/s and target angle of 45° to analyze the absolute error of JPS. Next, we applied the a muscle fatigue protocol, running 100 repetitions of isokinetic knee flexion-extension at 90°/s. Concurrently with this protocol, there was the assessment of muscle performance, as the peak torque (PT) and fatigue index, and electromyographic activity (RMS and median frequency). Finally, we repeated the assessment of JPS. The statistical analysis showed that patients after ACL reconstruction have, even under normal conditions, the amended JPS compared with healthy subjects and that after fatigue, both have disturbances in the JPS, but this alteration is significantly exacerbated in patients after ACL reconstruction. About muscle performance, we could notice that these patients have a lower PT, although there are no differences between the dynamometric and EMG fatigue index. These findings show the necessity about the cares of pacients with ACL reconstruction in respect of the risks of articulate instability and overload in ligamentar graft

Efeitos da eletroestimulação sobre os parâmetros eletromiográficos e dinamométricos do músculo quadríceps femoral

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

Influência do kinesio taping® no desempenho neuromuscular do quadríceps femoral e na função do membro inferior em sujeitos saudáveis: ensaio clínico, controlado, randomizado, cego

Objective:To analyze the immediate effects of the Kinesio Taping® application on the quadriceps neuromuscular performance, postural balance and lower limb function in healthy subjects. Materials andmethods:This is a randomized, controlled, blinded clinical trial. Sixtyfemale volunteers(age: 23.3±2.5 years old, BMI: 22.2±2.1kg/m2)wererandomly assigned intothreegroups with20memberseach,and performedone of these threeprotocols: control -10 minutesof rest,experimental 1- patch application ontherectusfemoris (RF), vastuslateralis(VL) and vastusmedialis(VM) and experimental 2-KT application on the same muscles. Allunderwent an evaluationfor singleand triple hop distance, postural balance (baropodometry), joint position sense(JPS), peak torque (concentric and eccentricevaluation at 60°/s)and electromyographic activityof VL,before andafter intervention.Results: There wasasignificant increasein the jump distanceof thethreestudied groups,with no differencebetween groups.There were nosignificant changesin postural balance,JPS, concentricpeak torqueand RMSof the VLin none of the groups. There was a reduction ineccentricpeak torquein all groups, without differencesbetween groups.Conclusion:The KT application on the RF, VL and VMmusclesis not able tosignificantly improvelower limbfunction and postural balance, as well as the kneeextensor peaktorque, JPSand the VL muscleactivation amplitudeof healthy women.

Efeito do tempo de repouso após fadiga induzida no desempenho neuromuscular do quadríceps femoral: ensaio clínico, controlado, randomizado, cego

Objective: To evaluate the effect of different resting periods, after induced muscle fatigue, in the quadriceps femoris neuromuscular performance, in healthy subjects. Methods: Sixty-four volunteers, of both genders, with an average of 21,8 ± 1,7 years and mean body mass index of 24,2 ± 3,7 Kg/m2 were randomly assigned into 4 groups: control group (was not induced fatigue); Experimental Group 1 (Exp. 1 1 minute of rest after fatigue); Experimental Group 3 (Exp. 3 3 minutes of rest after fatigue) and Experimental Group 5 (Exp. 5 5 minutes of rest after fatigue). The subjects were evaluated to the knee´s joint position sense (JPS), followed by 5 flexion-extension knee concentric isokinetic contractions at 60°/s, with concomitant recording of median frequency (Fmed) of rectus femoris (RF), vastus lateralis (VL) and vastus medialis (VM). Then they underwent a muscle fatigue protocol (30 flexion-extension knee concentric contractions at 60°/s) and were reevaluated on the isokinetic performance, Fmed and JPS. Blood lactate levels were measured before initial assessment, immediately after the fatigue protocol and 5 minutes after the end of the rest period. Results: The adoption of 3 minutes of rest was sufficient to restore the initial conditions for the peak torque normalized by body weight and the VL and VM Fmed. The joint position sense returned to its initial values with 1 minute rest. The lactate concentration remained high regardless of the adopted rest period. Conclusion: The use of 3-minute rest period is sufficient for the reestablishment of the neuromuscular parameters to the pre fatigue values.