Development of a dynamic headspace solid-phase microextraction procedure coupled to GC–qMSD for evaluation the chemical profile in alcoholic beverages

In the present study, a simple and sensitive methodology based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography with quadrupole mass detection (GC–qMSD), was developed and optimized for the determination of volatile (VOCs) and semi-volatile (SVOCs) compounds from different alcoholic beverages: wine, beer and whisky. Key experimental factors influencing the equilibrium of the VOCs and SVOCs between the sample and the SPME fibre, as the type of fibre coating, extraction time and temperature, sample stirring and ionic strength, were optimized. The performance of five commercially available SPME fibres was evaluated and compared, namely polydimethylsiloxane (PDMS, 100 μm); polyacrylate (PA, 85 μm); polydimethylsiloxane/divinylbenzene (PDMS/DVB, 65 μm); carboxen™/polydimethylsiloxane (CAR/PDMS, 75 μm) and the divinylbenzene/carboxen on polydimethylsiloxane (DVB/CAR/PDMS, 50/30 μm) (StableFlex). An objective comparison among different alcoholic beverages has been established in terms of qualitative and semi-quantitative differences on volatile and semi-volatile compounds. These compounds belong to several chemical families, including higher alcohols, ethyl esters, fatty acids, higher alcohol acetates, isoamyl esters, carbonyl compounds, furanic compounds, terpenoids, C13-norisoprenoids and volatile phenols. The optimized extraction conditions and GC–qMSD, lead to the successful identification of 44 compounds in white wines, 64 in beers and 104 in whiskys. Some of these compounds were found in all of the examined beverage samples. The main components of the HS-SPME found in white wines were ethyl octanoate (46.9%), ethyl decanoate (30.3%), ethyl 9-decenoate (10.7%), ethyl hexanoate (3.1%), and isoamyl octanoate (2.7%). As for beers, the major compounds were isoamyl alcohol (11.5%), ethyl octanoate (9.1%), isoamyl acetate (8.2%), 2-ethyl-1-hexanol (5.9%), and octanoic acid (5.5%). Ethyl decanoate (58.0%), ethyl octanoate (15.1%), ethyl dodecanoate (13.9%) followed by 3-methyl-1-butanol (1.8%) and isoamyl acetate (1.4%) were found to be the major VOCs in whisky samples.

Simultaneous analysis of free amino acids and biogenic amines in honey and wine samples using in loop orthophthalaldeyde derivatization procedure

This work presents a RP-HPLC method for the simultaneous quantification of free amino acids and biogenic amines in liquid food matrices and the results of the application to honey and wine samples obtained from different production processes and geographic origins. The developed methodology is based on a pre-column derivatization with o-phthaldialdehyde carried out in the sample injection loop. The compounds were separated in a Nova-Pack RP-C18 column (150 mm × 3.9 mm, 4 μm) at 35 °C. The mobile phase used was a mixture of phase A: 10 mM sodium phosphate buffer (pH 7.3), methanol and tetrahydrofuran (91:8:1); and phase B: methanol and phosphate buffer (80:20), with a flow rate of 1.0 ml/min. Fluorescence detection was used at an excitation wavelength of 335 nm and an emission wavelength of 440 nm. The separation and quantification of 19 amino acids and 6 amines was carried out in a single run as their OPA/MCE derivatives elute within 80 min, ensuring a reproducible quantification. The method showed to be adequate for the purpose, with an average RSD of 2% for the different amino acids; detection limits varying between 0.71 mg/l (Asn) and 8.26 mg/l (Lys) and recovery rates between 63.0% (Cad) and 98.0% (Asp). The amino acids present at the highest concentration in honey and wine samples were phenylalanine and arginine, respectively. Only residual levels of biogenic amines were detected in the analysed samples.

In situ differentiation of labile/inert metal species in Brazilian tropical rivers by means of a time-controlled batch-procedure based on TEPHA resin

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

A responsabilização criminal no estado democrático de direito: o equilíbrio entre a efetividade e os limites da pretensão punitiva da sociedade

This paper analyzes the relationship between fundamental rights and the exercise of the claim punitive society in a democratic state. It starts with the premise that there are fundamental rights that limit and determine the validity of all forms of manifestation of the claim punitive society (legislating, investigative, adjudicative or ministerial) and there are others that require the state the right exercise, fast and effective of these activities. Travels to history in order to see that the first meaning of these rights was built between the seventeenth and eighteenth centuries, after all a history of abuses committed by state agents in the exercise of criminal justice, and positively valued in the declarations of human rights and proclaimed in the constitutions after the American and French Revolutions, while the second meaning has been assigned between the nineteenth and twentieth centuries, when, because of the serious social problems generated largely by absenteeism state, it was noted that in addition to subjective rights the individual against the state, fundamental rights are also objective values, which trigger an order directed the state to protect them against the action of the offending individuals themselves (duty to protect), the mission of which the State seeks to discharge, among other means, through the issue of legal rules typifying the behavior detrimental to such rights, subject to penalties, and the concrete actions of public institutions created by the Constitution to operate penal law. Under this double bias, it is argued that the rule violates the Constitution in the exercise of the claim punitive society as much as by excess malfere fundamental rights that limit, as when it allows facts wrong by offending fundamental rights, remain unpunished either by inaction or by insufficient measures taken abstractly or concretely provided

Alternative procedure for the cold test for soybean seeds

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Treatment of PVC using an alternative low energy ion bombardment procedure

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

Efficient procedure to evaluate electromagnetic transients on three-phase transmission lines

This paper presents a hybrid way mixing time and frequency domain for transmission lines modelling. The proposed methodology handles steady fundamental signal mixed with fast and slow transients, including impulsive and oscillatory behaviour. A transmission line model is developed based on lumped elements representation and state-space techniques. The proposed methodology represents an easy and practical procedure to model a three-phase transmission line directly in time domain, without the explicit use of inverse transforms. The proposed methodology takes into account the frequency-dependent parameters of the line, considering the soil and skin effects. In order to include this effect in the state matrices, a fitting method is applied. Furthermore the accuracy of proposed the developed model is verified, in frequency domain, by a simple methodology based on line distributed parameters and transfer function related to the input/output signals of the lumped parameters representation. In addition, this article proposes the use of a fast and robust analytic integration procedure to solve the state equations, enabling transient and steady-state simulations. The results are compared with those obtained by the commercial software Microtran (EMTP), taking into account a three-phase transmission line, typical in the Brazilian transmission system.

Paulo Egídio e a sociologia criminal em São Paulo

Este artigo discute a trajetória intelectual e política de Paulo Egídio. Autor praticamente esquecido pelos trabalhos que reconstituem a história do pensamento social no Brasil, Paulo Egídio foi um importante divulgador da sociologia entre o final do século XIX e o início do século XX em São Paulo, tendo produzido uma obra pioneira sobre Durkheim e desenvolvido cursos livres da disciplina. O artigo busca também apresentar alguns aspectos de sua atividade política como senador nos primeiros momentos da República, quando teve destacada participação no debate sobre a criação de uma rede de instituições de controle social e, em particular, sobre a construção de uma nova penitenciária para o estado de São Paulo.

Códigos de sustentação da linguagem no cotidiano prisional do Rio Grande do Norte: penitenciária estadual de Parnamirim

The quarrel, in this study, tells about the language as social practical in the daily of Parnamirim State Prison that is integrated to the Rio Grande do Norte Penitentiary System - SISPERN, destined for men in fulfilment of penalty privative of freedom, in closed regimen. For the accomplishment of the research, the delimited objectives had been to analyze the language repertoires created in the prisional daily, trying to identify how it´s turned into distinct forms of resistance to the mechanisms of control in penitentiary system; to investigate which are the language repertoires created from the new sociability forms developed among prisoners and identify how the language repertoires are expressed in the daily prisional on relations/exercises of power not-institutionalized. In the methodological aspect, the study is in a qualitative boarding, that has as main instrument the interview. The inquiry was possible by means of using instruments for data collection, like as: the direct comment in the prisional daily duly registered as researcher´s ethnographical procedure, the analysis of interns´ cadastre handbooks and the application of half-structuralized interview, to the subjects of the research. The construction and understanding of the study object had been based on authors who argue on the arrest, as: Foucault, Goffman, Carvalho Filho and, in particular was searched the theorical referencial that approaches the language in a social and cultural perspective: Orlandi, Manfred, Bastos and Candiotto, amongst others. Beyond the normative endorsement of the Brazilian legislation, through the Law of Criminal Execution, of the Criminal Code and the Federal Constitution of the country and the legal apparatus in state scope. Still in the research methodological perspective, after the collection the data had been submitted to an analysis of the speech from Foucalt´s theory and in the Orlandi´s perspective, being also qualitative and quantitative. The results had evidenced that the social and juridical profile of the population in the site inquired is not different of others Brazilian prisons, composed for men, in its majority, with age band between 21 and 30 years old, prisoners for practicing crimes against the patrimony, against life, amongst others, and, in special, criminal recidivists. It evidenced, still, that the daily prisional of PSP is characterized for a sociocultural diversity expressed in the relations of power not institutionalized, that contributes for the formation and division of the groups, each one using a set of language codes/ repertoires sustentation. Therefore, the language, in the daily prisional, is one of the ways to understand the singularity of the sociability relations and as social practicing mediated by relations/exercises of power and antagonistic interests, in which each group aims first of all, their own interests. It represents the complexity of the social relations, in the prisional space, with diverse effects, in function of the situation and the moment. The language in the arrest, beyond the communication function, assumes and represents central element for the sociability human being, contributes for its changings and it´s configured as one of the resistance forms of prisoners against the controling, disciplining and monitoring mechanisms of penitentiary system

Typing class I HLA-A gene using a nested PCR-RFLP procedure

In order to detect several new HLA-A class I alleles that have been described since 1998, the original PCR-RFLP method developed to identify the 78 alleles recognized at that time at high resolution level was adapted by us for low and medium resolution levels using a nested PCR-RFLP approach. The results obtained from blood samples of 23 subjects using both the PCR-RFLP method and a commercial kit (MicroSSP1A®, One Lambda Inc.) showed an agreement higher than 95%. The PCR-RFLP adapted method was effective in low and medium resolution histocompatibility evaluations.

Analytical procedure based on slurry sampling for determining selenium in organic vegetable samples by graphite furnace atomic absorption spectrometry

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