Morfologia externa, composição corporal e performance motora do praticante de atletismo madeirense : um estudo em atletas dos 11-17 anos de idade

Os objetivos centrais da presente pesquisa foram quatro: (1) recolher informação nos domínios do crescimento físico humano, composição corporal, tipo físico, aptidão física e prática desportiva do atleta infanto-juvenil praticante de atletismo; (2) estudar a variação associada à idade e ao sexo; (3) investigar as diferenças entre atletas e não-atletas; e (4) identificar os preditores da capacidade funcional. A amostra foi constituída por 105 praticantes de atletismo, 49 do sexo masculino e 56 do sexo feminino, com idades compreendidas entre os 11 e os 17 anos, de cinco clubes da Região Autónoma da Madeira. As variáveis de estudo incluíram a altura, o peso corporal, os diâmetros ósseos, os perímetros musculares, as pregas de adiposidade subcutânea, a massa isenta de gordura (MIG), a massa gorda, o tipo físico, os testes motores, e os anos e as horas de treino semanal. Os ‘scores’ Z, os testes t-student e Mann-Whitney U, a ANOVA e a regressão linear múltipla foram os procedimentos estatísticos utilizados nas análises. O atleta do sexo masculino foi mais alto, pesado, robusto e apresentou mais MIG do que o sexo feminino (p<0,05). Os atletas apresentaram um físico mesomorfo equilibrado (sexo masculino) e meso-endomorfo (sexo feminino). Os rapazes apresentaram valores significativamente superiores na aptidão física geral e específica, comparativamente às raparigas. As raparigas apresentaram melhores desempenhos no ‘sit and reach’(p<0,05). Os valores médios para a altura, peso corporal, testes motores e características da prática desportiva foram superiores nas atletas mais velhas (p<0,05). Os praticantes de atletismo apresentaram menos gordura subcutânea e melhores desempenhos no salto em comprimento sem corrida preparatória e corrida de 12 minutos, do que as não-atletas. A altura, a percentagem de gordura, os anos de prática desportiva e o número de horas de treino por semana foram os preditores que mais contribuíram para explicar a variância nos testes motores.Os resultados demonstraram um dimorfismo entre atletas do sexo masculino e feminino. O treino estava associado a melhores desempenhos nos testes motores e a valores mais baixos de gordura corporal. A altura, a gordura corporal e as características da prática desportiva foram importantes na predição da capacidade funcional.

New method for determination of (E)resveratrol in wine based on microextraction using packed sorbent and ultra-performance liquid chromatography

An ultra-fast and improved analytical methodology based on microextraction by packed sorbent (MEPS) combined with ultra-performance LC (UPLC) was developed and validated for determination of (E)-resveratrol in wines. Important factors affecting the performance of MEPS such as the type of sorbent material (C2, C8, C18, SIL, and M1), number of extraction cycles, and sample volume were studied. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (50–250mL) in one extraction cycle (extract–discard) and in a short time period (about 3 min for the entire sample preparation step). (E)-Resveratrol was eluted by 1 250mL of the mixture containing 95% methanol and 5% water, and the separation was carried out on a highstrength silica HSS T3 analytical column (100 mm 2.1 mm, 1.8mm particle size) using a binary mobile phase composed of aqueous 0.1% formic acid (eluent A) and methanol (eluent B) in the gradient elution mode (10 min of total analysis). The method was fully validated in terms of linearity, detection (LOD) and quantification (LOQ) limits, extraction yield, accuracy, and inter/intra-day precision, using a Madeira wine sample (ET) spiked with (E)-resveratrol at concentration levels ranging from 5 to 60mg/mL. Validation experiments revealed very good recovery rate of 9575.8% RSD, good linearity with r2 values 40.999 within the established concentration range, excellent repeatability (0.52%), and reproducibility (1.67%) values (expressed as RSD), thus demonstrating the robustness and accuracy of the MEPSC8/UPLC-photodiode array (PDA) method. The LOD of the method was 0.21mg/mL, whereas the LOQ was 0.68mg/mL. The validated methodology was applied to 30 commercial wines (24 red wines and six white wines) from different grape varieties, vintages, and regions. On the basis of the analytical validation, the MEPSC8/UPLC-PDA methodology shows to be an improved, sensitive, and ultra-fast approach for determination of (E)-resveratrol in wines with high resolving power within 6 min.

A sensitive microextraction by packed sorbent-based methodology combined with ultra-high pressure liquid chromatography as a powerful technique for analysis of biologically active flavonols in wines

A new approach based on microextraction by packed sorbent (MEPS) and reversed-phase high-throughput ultra high pressure liquid chromatography (UHPLC) method that uses a gradient elution and diode array detection to quantitate three biologically active flavonols in wines, myricetin, quercetin, and kaempferol, is described. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (selectivity, linearity, sensitivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters such as the type of sorbent material (C2, C8, C18, SIL, and C8/SCX), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, on the MEPS performance. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250 μL) in five extraction cycle and in a short time period (about 5 min for the entire sample preparation step). Under optimized conditions, excellent linearity View the MathML source(Rvalues2>0.9963), limits of detection of 0.006 μg mL−1 (quercetin) to 0.013 μg mL−1 (myricetin) and precision within 0.5–3.1% were observed for the target flavonols. The average recoveries of myricetin, quercetin and kaempferol for real samples were 83.0–97.7% with relative standard deviation (RSD, %) lower than 1.6%. The results obtained showed that the most abundant flavonol in the analyzed samples was myricetin (5.8 ± 3.7 μg mL−1). Quercetin (0.97 ± 0.41 μg mL−1) and kaempferol (0.66 ± 0.24 μg mL−1) were found in a lower concentration. The optimized MEPSC8 method was compared with a reverse-phase solid-phase extraction (SPE) procedure using as sorbent a macroporous copolymer made from a balanced ratio of two monomers, the lipophilic divinylbenzene and the hydrophilic N-vinylpyrrolidone (Oasis HLB) were used as reference. MEPSC8 approach offers an attractive alternative for analysis of flavonols in wines, providing a number of advantages including highest extraction efficiency (from 85.9 ± 0.9% to 92.1 ± 0.5%) in the shortest extraction time with low solvent consumption, fast sample throughput, more environmentally friendly and easy to perform.

A new and improved strategy combining a dispersive-solid phase extraction-based multiclass method with ultra high pressure liquid chromatography for analysis of low molecular weight polyphenols in vegetables

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.

A fast method using a new hydrophilic–lipophilic balanced sorbent in combination with ultra-high performance liquid chromatography for quantification of significant bioactive metabolites in wines

This manuscript describes the development and validation of an ultra-fast, efficient, and high throughput analytical method based on ultra-high performance liquid chromatography (UHPLC) equipped with a photodiode array (PDA) detection system, for the simultaneous analysis of fifteen bioactive metabolites: gallic acid, protocatechuic acid, (−)-catechin, gentisic acid, (−)-epicatechin, syringic acid, p-coumaric acid, ferulic acid, m-coumaric acid, rutin, trans-resveratrol, myricetin, quercetin, cinnamic acid and kaempferol, in wines. A 50-mm column packed with 1.7-μm particles operating at elevated pressure (UHPLC strategy) was selected to attain ultra-fast analysis and highly efficient separations. In order to reduce the complexity of wine extract and improve the recovery efficiency, a reverse-phase solid-phase extraction (SPE) procedure using as sorbent a new macroporous copolymer made from a balanced ratio of two monomers, the lipophilic divinylbenzene and the hydrophilic N-vinylpyrrolidone (Oasis™ HLB), was performed prior to UHPLC–PDA analysis. The calibration curves of bioactive metabolites showed good linearity within the established range. Limits of detection (LOD) and quantification (LOQ) ranged from 0.006 μg mL−1 to 0.58 μg mL−1, and from 0.019 μg mL−1 to 1.94 μg mL−1, for gallic and gentisic acids, respectively. The average recoveries ± SD for the three levels of concentration tested (n = 9) in red and white wines were, respectively, 89 ± 3% and 90 ± 2%. The repeatability expressed as relative standard deviation (RSD) was below 10% for all the metabolites assayed. The validated method was then applied to red and white wines from different geographical origins (Azores, Canary and Madeira Islands). The most abundant component in the analysed red wines was (−)-epicatechin followed by (−)-catechin and rutin, whereas in white wines syringic and p-coumaric acids were found the major phenolic metabolites. The method was completely validated, providing a sensitive analysis for bioactive phenolic metabolites detection and showing satisfactory data for all the parameters tested. Moreover, was revealed as an ultra-fast approach allowing the separation of the fifteen bioactive metabolites investigated with high resolution power within 5 min.

Morfologia, performance e fatores contextuais do nadador salvador infanto-juvenil madeirense

O objetivo central do presente estudo foi triplo: (1) reunir a bibliografia existente sobre o nadador infanto-juvenil; (2) avaliar a estrutura, a composição corporal e a aptidão física geral e específica do nadador infanto-juvenil madeirense e (3) investigar as relações entre o crescimento físico humano, a aptidão física e as variáveis contextuais. A amostra incluiu 97 nadadores, 46 do sexo masculino e 51 do sexo feminino, 11-16 anos, que integravam 4 clubes de Natação Pura Desportiva da Região Autónoma da Madeira. A altura, o peso corporal, a envergadura, os diâmetros ósseos, os comprimentos e larguras, os perímetros musculares e as pregas de adiposidade subcutânea foram medidos. A aptidão física geral e específica, a atividade física, o estatuto socioeconómico (ESE) e a prática desportiva foram quantificados. O teste t, o teste de Mann-Whitney U, o teste para a diferença entre duas proporções independentes e a análise de regressão múltipla foram utilizados na análise estatística dos dados. Os nadadores apresentaram valores médios mais elevados do que as nadadoras na altura, peso corporal, envergadura, comprimento e/ou largura dos segmentos e na quase totalidade dos diâmetros ósseos e perímetros musculares. As nadadoras apresentaram valores médios mais elevados do que os nadadores nas pregas de adiposidade subcutânea. Os nadadores apresentaram mais massa isenta de gordura do que as nadadoras. O tipo físico do nadador foi mesomorfo equilibrado (3,2-4,6-3,1) e o da nadadora endo-mesomorfo (4,3-3,5-2,9). Os nadadores apresentaram desempenhos mais elevados na quase totalidade dos testes motores. As nadadoras foram mais proficientes no ‘sit and reach’. As nadadoras, 14-16 anos, apresentaram valores médios mais elevados no peso corporal, envergadura, diâmetro biacromial, percentagem de gordura, batimento em placas, ‘sit ups’, anos de prática formal e total de horas de treino semanal, comparativamente aos 11-13 anos. As nadadoras foram, também, mais altas e pesadas, aos 11-13 anos, do que as não-atletas. A idade, o rácio envergadura/altura, a percentagem de gordura corporal, o ‘sit and reach’, o salto em comprimento sem corrida preparatória, os ‘sit ups’, o ‘shuttle run’, a corrida de 12 minutos, o índice dos tempos livres e o total de competições nacionais por época desportiva explicaram 75,9% da variância no teste de nado de 12 minutos. Os resultados demonstraram um diferencial morfofuncional em função do sexo, idade e população de estudo. Os preditores do teste de nado de 12 minutos foram os indicadores de crescimento físico humano, a aptidão física e as variáveis contextuais.