Influência do método de extração nos teores de metilxantinas em erva-mate (Ilex paraguariensis a. St.-Hil., aquifoliaceae)

Ilex paraguariensis A. St. -Hil. is a native species of southern South America. The caffeine content in Ilex paraguariensis leaves has been considered an important quality parameter for maté-derived products. In this work different extraction methods for the determination of these methylxantines are compared. The influence of the extraction conditions on the methylxanthine yields was evaluated. Extraction by decoction with acidic aqueous solution (H2SO4 4N) presented the higher efficiency in the theobromine extraction. The extraction in a Soxhlet with acidic aqueous solution and decoction with acidic aqueous solution showed the highest caffeine yield. For the concomitant theobromine and caffeine quantification, the decoction with acidic aqueous solution is suggested.

Determinação de açúcar total em café cru por espectroscopia no infravermelho próximo e regressão por mínimos quadrados parciais

In this work a fast method for the determination of the total sugar levels in samples of raw coffee was developed using the near infrared spectroscopy technique and multivariate regression. The sugar levels were initially obtained using gravimety as the reference method. Later on, the regression models were built from the near infrared spectra of the coffee samples. The original spectra were pre-treated according to the Kubelka-Munk transformation and multiplicative signal correction. The proposed analytical method made possible the direct determination of the total sugar levels in the samples with an error lower by 8% with respect to the conventional methodology.

Otimização e validação da técnica de extração líquido-líquido com partição em baixa temperatura (ELL-PBT) para piretróides em água e análise por CG

The liquid-liquid extraction with the low temperature partition technique was developed for the analysis of four pyrethroids in water by CG. Using a factorial design the extraction technique was optimised evaluating the effect of the variables ionic strength, contact time and proportion between sample and solvent volumes. The validation parameters sensitivity, precision, accuracy and detection and quantification limits were evaluated. The LOD and LOQ of the method varied from 1.1 to 3.2 µg L-1 and 2.7 to 9.5 µg L-1, respectively.

Utilização da extração em fase sólida (SPE) na determinação de hidrocarbonetos policíclicos aromáticos em matrizes aquosas ambientais

Polycyclic aromatic hydrocarbons (PAHs) are a great environmental concern mainly because of their toxic, mutagenic and carcinogenic potential. This paper reports utilization of the solid-phase extraction (SPE) technique to determine PAHs in environmental aqueous matrices. The recovery from environmental aqueous matrices fortified with PAHs varied from 63.7 to 93.1% for atmospheric liquid precipitation, from 38.3 to 95.1% for superficial river water, and from 71.0 to 95.5% for marine water. No negative matrix effect was observed for the recovery of PAHs from atmospheric liquid precipitation and marine water, but was observed for superficial river water, particularly for PAHs possessing 5 and 6 aromatic rings.

Influência do processamento e da torrefação sobre a atividade antioxidante do café (Coffea arabica)

The aim of this work is to evaluate the influence of processing (semi-dry and dry) and roasting (light, medium and dark) on the antioxidant activity of coffee brews, using tests to determine the reducing power and the DPPH scavenging, Fe+2 chelating and lipid peroxidation inhibition activities. All of the coffee brews presented concentration-dependent antioxidant activity. The light coffee samples presented the higher reducing power and DPPH scavenging activity. Its ion chelating capacity was similar to the medium samples, but was less than the green coffee chelating capacity. The semi-dry processing was more efficient than the dry processing only for the reducing power. All of the samples presented high lipid peroxidation inhibition activity. Based on the results the degree of coffee roasting seems to be more important than the processing to determine the antioxidant activity of brews.

Extração, estruturas e propriedades de alfa- e beta-quitina

The fact that alpha- and beta-chitin adopt different arrays in the solid state is explored to emphasize their different properties and distinct spectral characteristics and X ray diffraction patterns. The methods for their extraction from the biomass in view of the preservation of their native structures and aiming to fulfill the claims of purity and uniformity for potential applications are discussed. The different arrays adopted by alpha- and beta-chitin also result in distinct reactivities toward the deacetylation reaction. Thus, the deacetylation of beta-chitin is more efficient owing to the better accessibility to amide groups due to the lower crystallinity of this polymorph.

Recuperação de cádmio de baterias níquel-cádmio via extração seletiva com tributilfosfato (TBP)

This work describes a recovery process of cadmium from spent nickel-cadmium batteries by a new hydrometallurgical route based on the selective extraction in hydrochloric acid medium with tributylphosphate (TBP), alone or dissolved in kerosene. The best results were obtained when TBP concentration was at least 75 vol%. Nickel extraction was negligible under these conditions. It was isolated after processing the rafinate through an anionic ion-exchange column. Final wastes generated are basically sodium chloride solutions, with no turbidity, color or heavy metals present in significant amounts.

Determinação do coeficiente de atividade na diluição infinita (g¥) através da micro-extração em fase sólida (SPME)

In this study a new approach, solid phase micro extraction (SPME), is used in the evaluation of the infinite dilution activity coefficient of the solute in a given solvent. It is the purpose of the current work to demonstrate a different approach to obtain the data needed for studying the solution thermodynamics of binary liquid mixtures as well as for designing multi-component separations. The solutes investigated at the temperature 298.15 K were toluene, ethyl benzene and xylene in the solvent methanol.

Métodos de extração para quantificação de manganês disponível em fertilizantes

The solubility of Mn in different fertilizers (MnSO4.H2O-p.a., MnO2-p.a.+MnO-Ind., MnO2-Ind.+MnO-Ind., MnO2-p.a., MnO2-Ind. and MnO-Ind.) was determined using different methodologies: total content and soluble contents in water, 10% H2SO4, citric acid at 20 g L-1, diluted neutral ammonium citrate, (1+9) and DTPA at 0.005 mol L-1. The Mn solubilities in the latter three extractors were assessed after agitation of the sample for one hour and after boiling for 5 minutes. The extraction procedure using neutral ammonium citrate (1+9), at 1:100, with agitation for one hour, was shown to be the most adequate to assess the availability of Mn in fertilizers.

Emprego de planejamento fatorial no desenvolvimento de uma metodologia para extração de zinco de resíduos galvânicos

The plating process generates solid waste rich in heavy metals and aiming to reduce environmental impact of such waste, this work suggests a methodology for zinc reduction, through a 2(4) factorial planning, studying the influence of the following variables: acid concentration (15, 20 or 30% v/v), acid type (sulfuric or hydrochloric), acid volume (15, 20 or 25 mL) and extraction time (12, 24 or 36 h). Through this methodology it is possible to establish the optimal conditions (15 mL of a 30% hydrochloric acid concentration during 12 h) to get a 100% efficiency in zinc extraction.

O enfoque da metrologia química em análises toxicológicas na atividade turfística: validação de método analítico para determinação de cafeína em matrizes biológicas

This paper proposes an alternate method to detect forbidden doping substances present in biological matrices of horseracing. The method was fully validated for caffeine, identified as the most frequent forbidden substance in the analysis conducted by the Antidoping Laboratory of the Brazilian Jockey Club, which adopts a zero threshold limit according to national and international horseracing practices. The metrological reliability of the method applied to toxicological analysis in biological matrices is discussed. Although the analytical method proposed for detection of a zero threshold level of the doping substance is qualitative, it was validated for the determination of the limiting value (also known as quantification limit value) introducing a criterion that prevents the issuing of incorrect results ("false-positives" and "false-negatives").

Utilização do índice de retenção linear para caracterização de compostos voláteis em café solúvel utilizando GC-MS e coluna HP-Innowax

Gas chromatography coupled with mass spectrometry (GC-MS) is widely used for the characterization of volatile compounds. However, due to the complexity of the soluble coffee matrix, a complete identification of the components should not be based on mass spectra interpretation only. The linear index of retention (LRI) is frequently used to give support to mass spectra. The aim of this work is to investigate the characterization of the volatile compounds in soluble coffee samples by GC-MS using LRI values found with a HP-INNOWAX column. The method used allows a significant increase of the reliability of identifying compounds.

Ondas ultrassônicas e pérolas de vidro: um novo método de extração de beta-galactosidase para uso em laboratório

The optimization of a traditional technique of cellular disruption by abrasion was carried out and a process using ultrasonic waves associated with glass pearls to extract beta-galactosidase from Kluyveromyces marxianus proposed. In the first case, the effects of the diameter and weight of the pearls in relation to the volume of cellular suspension and amount of time for cellular disruption were evaluated. The efficiency of the new process of cellular disruption was evaluated by varying the length of time of sonification and comparing with the method of abrasion under the same conditions. The proposed method can be efficiently applied to obtain beta-galactosidase at laboratory scale.

Preparação e caracterização de carvão ativado produzido a partir de resíduos do beneficiamento do café

Coffee fruit processing is one of the most polluting activities in agriculture due to the large amount of waste generated in the process. In this work, coffee parchment was employed as precursor for the production of carbons activated with ZnCl2 (CAP). The material was characterized using N2 adsorption/desorption at 77 K, Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The material showed a surface area of 521.6 m²g-1 and microporous structure. CAP was applied as adsorbent for the removal of methylene blue dye in aqueous medium. The adsorption capacity was found to be about 188.7 mg g-1.

Extração líquido-líquido de ferro(III) e titânio(IV) pelo ácido bis-(2-etil-hexil) fosfórico (D2EHPA) em meio de ácido sulfúrico

This work presents a study on the separation of Fe(III) and Ti(IV) from sulfuric acid leaching solutions of ilmenite (FeTiO3) using liquid-liquid extraction with D2EHPA in n-dodecane as extracting agent. The distribution coefficients (K D) of the elements related to free acidity and concentration of Fe(III) and Ti(IV) were determined. Free acidity was changed from 3x10-2 to 11.88 mol L-1 and D2EHPA concentration was fixed at 1.5 mol L-1. Recovery of final products as well as recycling of wastes generated in the process were also investigated. The LLE process as a feasible alternative to obtain high-purity TiO2.