Potentialities of two solventless extraction approaches—Stir bar sorptive extraction and headspace solid-phase microextraction for determination of higher alcohol acetates, isoamyl esters and ethyl esters in wines

A stir bar sorptive extraction with liquid desorption followed by large volume injection coupled to gas chromatography–quadrupole mass spectrometry (SBSE-LD/LVI-GC–qMS) was evaluated for the simultaneous determination of higher alcohol acetates (HAA), isoamyl esters (IsoE) and ethyl esters (EE) of fatty acids. The method performance was assessed and compared with other solventless technique, the solid-phase microextraction (SPME) in headspace mode (HS). For both techniques, influential experimental parameters were optimised to provide sensitive and robust methods. The SBSE-LD/LVI methodology was previously optimised in terms of extraction time, influence of ethanol in the matrix, liquid desorption (LD) conditions and instrumental settings. Higher extraction efficiency was obtained using 60 min of extraction time, 10% ethanol content, n-pentane as desorption solvent, 15 min for the back-extraction period, 10 mL min−1 for the solvent vent flow rate and 10 °C for the inlet temperature. For HS-SPME, the fibre coated with 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) afforded highest extraction efficiency, providing the best sensitivity for the target volatiles, particularly when the samples were extracted at 25 °C for 60 min under continuous stirring in the presence of sodium chloride (10% (w/v)). Both methodologies showed good linearity over the concentration range tested, with correlation coefficients higher than 0.984 for HS-SPME and 0.982 for SBES-LD approach, for all analytes. A good reproducibility was attained and low detection limits were achieved using both SBSE-LD (0.03–28.96 μg L−1) and HS-SPME (0.02–20.29 μg L−1) methodologies. The quantification limits for SBSE-LD approach ranging from 0.11 to 96.56 μg L−and from 0.06 to 67.63 μg L−1 for HS-SPME. Using the HS-SPME approach an average recovery of about 70% was obtained whilst by using SBSE-LD obtained average recovery were close to 80%. The analytical and procedural advantages and disadvantages of these two methods have been compared. Both analytical methods were used to determine the HAA, IsoE and EE fatty acids content in “Terras Madeirenses” table wines. A total of 16 esters were identified and quantified from the wine extracts by HS-SPME whereas by SBSE-LD technique were found 25 esters which include 2 higher alcohol acetates, 4 isoamyl esters and 19 ethyl esters of fatty acids. Generally SBSE-LD provided higher sensitivity with decreased analysis time.

In-depth search focused on furans, lactones, volatile phenols, and acetals as potential age markers of Madeira wines by comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction

The establishment of potential age markers of Madeira wine is of paramount significance as it may contribute to detect frauds and to ensure the authenticity of wine. Considering the chemical groups of furans, lactones, volatile phenols, and acetals, 103 volatile compounds were tentatively identified; among these, 71 have been reported for the first time in Madeira wines. The chemical groups that could be used as potential age markers were predominantly acetals, namely, diethoxymethane, 1,1-diethoxyethane, 1,1-diethoxy-2-methyl-propane, 1-(1-ethoxyethoxy)-pentane, trans-dioxane and 2-propyl-1,3-dioxolane, and from the other chemical groups, 5-methylfurfural and cis-oak-lactone, independently of the variety and the type of wine. GC × GC-ToFMS system offers a more useful approach to identify these compounds compared to previous studies using GC−qMS, due to the orthogonal systems, that reduce coelution, increase peak capacity and mass selectivity, contributing to the establishment of new potential Madeira wine age markers. Remarkable results were also obtained in terms of compound identification based on the organized structure of the peaks of structurally related compounds in the GC × GC peak apex plots. This information represents a valuable approach for future studies, as the ordered-structure principle can considerably help the establishment of the composition of samples. This new approach provides data that can be extended to determine age markers of other types of wines.

Optimisation of solid-phase microextraction combined with gas chromatography–mass spectrometry based methodology to establish the global volatile signature in pulp and skin of Vitis vinifera L. grape varieties

The volatiles (VOCs) and semi-volatile organic compounds (SVOCs) responsible for aroma are mainly present in skin of grape varieties. Thus, the present investigation is directed towards the optimisation of a solvent free methodology based on headspace-solid-phase microextraction (HS-SPME) combined with gas chromatography–quadrupole mass spectrometry (GC–qMS) in order to establish the global volatile composition in pulp and skin of Bual and Bastardo Vitis vinifera L. varieties. A deep study on the extraction-influencing parameters was performed, and the best results, expressed as GC peak area, number of identified compounds and reproducibility, were obtained using 4 g of sample homogenised in 5 mL of ultra-pure Milli-Q water in a 20 mL glass vial with addition of 2 g of sodium chloride (NaCl). A divinylbenzene/carboxen/polydimethylsiloxane fibre was selected for extraction at 60 °C for 45 min under continuous stirring at 800 rpm. More than 100 VOCs and SVOCs, including 27 monoterpenoids, 27 sesquiterpenoids, 21 carbonyl compounds, 17 alcohols (from which 2 aromatics), 10 C13 norisoprenoids and 5 acids were identified. The results showed that, for both grape varieties, the levels and number of volatiles in skin were considerably higher than those observed in pulp. According to the data obtained by principal component analysis (PCA), the establishment of the global volatile signature of grape and the relationship between different part of grapes—pulp and skin, may be an useful tool to winemaker decision to define the vinification procedures that improves the organoleptic characteristics of the corresponding wines and consequently contributed to an economic valorization and consumer acceptance.

Prevalência de oclusopatias e caracteríticas cefalométricas e dentais de escolares cearense da cidade de Fortaleza

The people of Ceará state are descended from miscegenation between the Portuguese colonizers and the native population, resulting in a different facial pattern from other populations. It is important that this pattern be thoroughly understood, along with its minimum and maximum values so that they can be assessed and respected, allowing professionals who deal with the craniofacial complex to work more efficiently and scientifically. Aim: To characterize the morphological pattern of individuals from Ceará state, whose father and grandfather are also native from Ceará, in the 10-12 year age group, not submitted to previous orthodontic treatment, in order to determine: 1) the prevalence of occlusal pattern; 2) the prevalence of dental anomalies (DA) and, 3) the skeletal and dental cephalometric characteristics of individuals that present with normal occlusion and harmonious facial pattern. Methodology: A list of 10-12 year-olds was obtained from 515 schools containing 162,713 students (Education Secretariat of Ceará State), from which 234 individuals were examined (107 boys and 157 girls). The assessment criteria adopted were: 1) Angle s Classification System to determine occlusal pattern. The occlusal characteristics were measured through overbite, overjet, crowding and interincisal diastema. 2) DA are anomalies of number, shape, size, eruption and structure and, 3) in the group that presented with normal occlusion, we used cephalometric analysis measures proposed by Downs, Steiner, Tweed, Holdaway, Jacobson and McNamara. Results: 1) 25.8% of the schoolchildren had normal occlusion, 47.5% class I malocclusion, 22.3% class II malocclusion and 4.2% class III malocclusion. No statistically significant difference was found between the age group studied and sex. Thirty percent of the individuals had normal overbite, while 36.7% and 19.7% had increased and reduced overbite, respectively. Normal overjet was found in 33.7% of the individuals, increased overjet in 50% and reduced in 16.3%. Dental crowding was observed in 62.5% of the individuals and the presence of interincisal diastema in 14.8%. 2) The prevalence of DA was 56.1%, 6.8% in the number, 10.8% in shape, 4.1% in size, 34.5% in eruption, 26.4% in structure and 17.4% had more than one DA. No association was found between DA and sex, but DA was significantly associated to malocclusion (p<0.05); 3) there was no association between sex or facial type between the measures of nasal-labial angle, position and effective maxillary length, effective mandibular length and the sagittal relationship between the molars, overjet and overbite, position of upper incisors, lower incisors and between the incisors themselves. There was a difference between sex, on the VERT index and in lower anterior facial height, upper incisor inclination and line-H, between facial types for the occlusal plane angles, mandibular plane, facial axis, lower incisor inclination, mandibular position, upper incisor position, lower anterior facial height, ANB and line-H. It was concluded that: 1) the most prevalent occlusal type was class I malocclusion, with no distinction for sex or age group, and the assessment of occlusal characteristics showed that excessive overbite and overjet were the most predominant findings, along with a high occurrence of tooth crowding; 2) a high prevalence of DA was found, particularly eruption anomalies, not influenced by sex but significantly associated to malocclusion and 3) individuals from Ceará are predominantly brachyfacial, exhibiting a number of similarities inherent to their facial pattern, such as a convex profile, retracted jaw, reduced lower third and protruded lower incisors. This study was multidisciplinary, involving researchers from the areas of epidemiology, radiology and dentistry, thereby meeting the multidisciplinarity requirements of the Postgraduate Program in Health Sciences

Mineralização de carbono e de nitrogênio provenientes de composto de lixo urbano em argissolo

Estudos da mineralização do C e do N em solos que receberam aplicação de composto de lixo urbano são importantes para avaliar o comportamento desse resíduo no solo e dar subsídios para definir as doses adequadas às culturas, com vistas em atender à necessidade de N das plantas. Foram realizados dois experimentos em condições de laboratório com o objetivo de avaliar a mineralização de C e de N em um Argissolo textura média adubado com composto de lixo urbano. No primeiro experimento, utilizou-se delineamento inteiramente ao acaso, com cinco tratamentos e três repetições, com os tratamentos constituídos de cinco doses de composto de lixo urbano, equivalentes a 0, 30, 60, 90 e 120 t ha-1. No segundo experimento, empregou-se esquema fatorial, com delineamento inteiramente ao acaso e três repetições, combinando as mesmas cinco doses de composto de lixo urbano utilizadas no primeiro experimento e 11 tempos de incubação (0, 7, 14, 28, 42, 56, 70, 84, 98, 112 e 126 dias). Os maiores aumentos de N-NO3- no solo foram obtidos até os 42 dias de incubação, independentemente da dose de composto de lixo aplicada, percebendo-se, a partir dos 70 dias, tendência de estabilização. A fração de mineralização de C-orgânico em C-CO2 menor do que 2 % em 168 dias indica que o composto de lixo urbano é material que contribui para aumentar os estoques de matéria orgânica do solo. Na ausência de adubação nitrogenada complementar, a fração de mineralização de N-orgânico de 12 % em 126 dias evidencia que o composto de lixo urbano apresenta potencial fertilizante de liberação lenta de N para as plantas.

Alterações nos atributos de fertilidade em solo adubado com composto de lixo urbano

O composto de lixo urbano é um adubo orgânico que vem sendo, com bastante freqüência, utilizado em áreas de produção de hortaliças. Assim, o objetivo deste trabalho foi avaliar o efeito da aplicação do composto de lixo urbano na fertilidade do solo, na produção de alface e no acúmulo de nutrientes nas plantas. O experimento foi realizado em casa de vegetação, em colunas de PVC, em delineamento em blocos ao acaso, com cinco tratamentos, doses de 0; 30; 60; 90 e 120 t ha-1 de composto de lixo urbano e oito repetições. As colunas receberam solo das profundidades de 0-20 (tratado com composto de lixo), 20-40 e 40-60 cm de um Argissolo, textura média, e uma muda de alface. Ao final do cultivo, colunas de quatro repetições de cada tratamento foram desmontadas e, nas demais colunas, fez-se um segundo cultivo de alface. A incorporação de composto de lixo urbano na profundidade de 0-20 cm melhorou a fertilidade do solo da própria camada em que foi aplicado e da camada de 20-40 cm, mas não alterou as características da camada de 40-60 cm. A adubação com composto de lixo urbano propiciou aumento do pH e dos teores de MO, P, K, Ca e Mg do solo, na camada de 0-20 cm, e de pH e Ca, na profundidade de 20-40 cm. A melhora da fertilidade do solo com a aplicação de composto de lixo urbano acarretou aumento de produção de alface e provocou maior acúmulo de P, K e Ca nas plantas.

Níveis de irrigação e de composto de lixo orgânico na formação de mudas cítricas em casa de vegetação

O presente trabalho visou a estudar o efeito da associação entre a irrigação e tipos de substratos na formação de mudas de laranjeira. O delineamento experimental utilizado foi o de blocos casualizados, com parcelas subdivididas, com quatro repetições, três níveis de irrigação e cinco tipos de substratos. Foram utilizados os seguintes substratos: 100% de casca de pínus; 80% de casca de pinus + 20% de composto de lixo orgânico; 60% de casca de pinus + 40% de composto de lixo orgânico; 20% de casca de pinus + 80% de composto de lixo orgânico, e 100% de composto de lixo orgânico. A irrigação por gotejamento foi feita com lâminas de 50%, 100% e 150% da evaporação do atmômetro modificado. A avaliação do desenvolvimento das plantas foi feita quinzenalmente, medindo-se o diâmetro do caule e a altura. Os resultados mostraram que as mudas de citrus apresentaram necessidade de água variável com os diferentes estádios de desenvolvimento e tipos de substratos, dos quais se destacou o substrato 3 (60% de casca de pinus e 40% de composto de lixo urbano), pois propiciou melhores condições para o desenvolvimento das raízes das plantas e também forneceu nutrientes, por meio da decomposição do material orgânico. A irrigação 3 (150% da evaporação do atmômetro) foi a que proporcionou o melhor desenvolvimento das mudas de laranjeira.

Biological control of Bradysia matogrossensis (Diptera : Sciaridae) in mushroom cultivation with predatory mites

Larvae of Sciaridae flies (Diptera) cause considerable damage to the mushroom Agaricus blazei (Murrill) ss. Heinemann in Brazil. Brazilian growers have had considerable difficulties in controlling this pest. The objective of this work was to test the effect of the predatory Laelapidae mite Stratiolaelaps scimitus (Womersley) as a control agent of Bradysia matogrossensis (Lane) in cultures of A. blazei. The work corresponded to an evaluation of the efficiency of that predator when released in boxes containing each about 15 L of commercial mushroom compost naturally infested with the pest. The results showed a significant effect of that predator on the population of B. matogrossensis. The release of either 665 or 1330 S. scimitus per box significantly reduced the pest population to levels that, according to grower's experience, apparently could not cause considerable damage. The positive results obtained warrant the conduction of complementary studies to determine the lowest rates of the predator that could still produce acceptable levels of control.

Seedlings production of Tabebuia heptaphylla in different substrates and levels of irrigation, in greenhouse conditions

The objective of this research was to evaluate the growth of Tabebuia heptaphylla seedlings in distinct substrates with different amounts of urban waste compost and the relation between this growth and irrigation. A completely randomized experimental design was used, with a factorial arrangement of 15 substrates and 2 irrigation levels. The substrates were composed by the combination of different materials: urban waste, tanned cattle manure, vermiculite, soil and the commercial form Plantmax (R). For the study of the seedlings development, the following characteristics were evaluated: plant height, stem diameter at soil level, number of leaves, above ground dry matter, root system dry matter, relation between plant height and stem base diameter, Dickson quality index and relation between plant height and above ground dry matter. Evaluations of plant height, stem diameter at soil level and number of leaves were made at 75, 90, 105, 120, 135 and 150 days after sowing. According to the results, it was concluded that urban waste compost does not increase plant development. Significant differences in relation to the irrigation levels were found, with better results for the 150% irrigation level compared to 100% evapotranspiration.

Adubação nitrogenada em cobertura e substratos na produção de mudas de mamoeiro 'Formosa'

Objetivando-se avaliar a produção de mudas de mamoeiro em diferentes substratos com adubações de nitrogênio em cobertura, conduziu-se um experimento em viveiro de formação de mudas no pomar da Universidade Federal de Lavras (UFLA), Minas Gerais. Foram testadas cinco doses de nitrogênio 0; 400; 800; 1600 e 3200 mg de N dm-3 de substrato, aplicados cinco vezes, sendo que em cada aplicação foram adicionados aos sacos de polietileno (capacidade de 500 mL) 20 mL de solução contendo o N e duas composições de substratos: A (composto orgânico + areia + solo na proporção de 1:1:3 em volume) e B (Plantmax® + areia + solo na proporção de 1:1:3 em volume). Foi utilizado o delineamento experimental em blocos ao acaso em esquema fatorial 5 x 2, com 4 repetições e cinco plantas por parcela. Após 150 dias da semeadura avaliaram-se as seguintes variáveis: comprimento da parte aérea (cm); comprimento de raiz (cm), número de folha/muda, matéria seca da parte aérea, da raiz e total (g/planta). Verificou-se que dosagem de até 1.800 mg de N dm-3 em cobertura, foram as que proporcionaram melhor qualidade na formação das mudas. em relação aos substratos verificou-se que o substrato B (Plantmax® + areia + solo na proporção de 1:1:3 em volume) foi o que promoveu os melhores resultados na produção das mudas do mamoeiro 'Formosa'.

Emergência e crescimento inicial de plântulas de pimenta ornamental e celosia em substrato à base de composto de lodo de curtume

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Análise da influência da qualidade em um ciclo de serviços na satisfação do cliente: estudo de caso em uma instituição de ensino.

With the increasing offer of education services in Brazil, it is necessary to evaluate the quality of service in education, especially in those institutions for vocational education which have a greater interaction with the labor market, in order to form qualified professionals and meet the growing demand that the country has today[A1] . In Brazil, the evaluation of the quality of library services has influenced the assessment of educational institutions and in this context, there needs to be a process to monitor the quality of services provided by libraries. However, the service is not done in a single moment and thus to a more detailed assessment it needs to be measured and evaluated each different time the customer uses it. Therefore, the aim of this work consists in measuring the quality in every moment of truth of a cycle of library services to assess which are the most relevant moments in the client's perspective at the library of the Federal Institute of Education, Science and Technology of Rio Grande do Norte (IFRN) Campus João Câmara in building the overall quality of service. In the literature review, internal secondary sources were used, from the database of the institution studied, and also external sources, through literature in books, articles, dissertations, theses and journals on compost quality, service quality, cycle services, measuring quality, satisfaction, teaching activities, and on library services specifically. We applied a questionnaire to students in the library based on models of quality measurement SERVPERF and SERVQUAL and its variations such as SERVQUAL pondered and SERVPERF pondered . Through analysis based on concepts of reliability and validity of measuring instruments, it was found that the SERVPERF model is the instrument that most closely matches the dimensions of quality assessed in the library with customer satisfaction measured by the questionnaire. From there, the search results as measured by statistical techniques of analysis, indicated that the initial and final moments of truth of the cycle of service quality had the greatest influence on overall customer satisfaction with the library service

Alterações em propriedades do solo adubado com composto orgânico e efeito na qualidade das sementes de alface

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

Alterações em propriedades de solo adubado com doses de composto orgânico sob cultivo de bananeira

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

Avaliação nutricional em folhas de bananeira 'Prata-anã' adubadas com composto orgânico

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