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.

Microextração em fase líquida (LPME): fundamentos da técnica e aplicações na análise de fármacos em fluidos biológicos

The analysis of drugs and metabolites in biological fluids usually requires extraction procedures to achieve sample clean-up and analyte preconcentration. Commonly, extraction procedures are performed using liquid-liquid extraction or solid-phase extraction. Nevertheless, these extraction techniques are considered to be time-consuming and require a large amount of organic solvents. On this basis, microextraction techniques have been developed. Among them, liquid-phase microextraction has been standing out. This review describes the liquid-phase microextraction technique based on hollow fibers as a novel and promising alternative in sample preparation prior to chromatographic or electrophoretic analysis. The basic concepts related to this technique and its applicability in extraction of drugs are discussed.

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.

Extração de β-caroteno de cenouras: uma proposta para disciplinas experimentais de química

This paper reports on the development of a simple and fast procedure for β-carotene extraction from carrots and its quantification by UV/Vis spectroscopy. Carotenoids extracted from carrots may also be used as alternative reagents for TLC (thin layer chromatography) detection of natural compounds with antioxidant properties, replacing the commercial p.a. grade β-carotene. Although this reagent had around 10% b-carotene, it proved to be as efficient for TLC analysis as the commercial p.a. grade β-carotene. This practice is a useful alternative for teaching undergraduate organic chemistry laboratory classes.

Avaliação do potencial antioxidante de extratos ativos de plantas obtidos por extração com fluido supercrítico

The aim of this work was to evaluate the antioxidant properties of ginger and rosemary extracts, obtained by supercritical extraction. The extracts were characterized by HPLC, GC-MS, phenolic compounds content and antioxidant activity. The main active compounds were identified and high content of phenolic compounds was observed. The extracts presented high antioxidant activity against the free radicals ABTS•+ (350 and 200 mM Trolox/g, for ginger and rosemary, respectively) and DPPH•+ (145 and 80 mM Trolox/g, for ginger and rosemary, respectively). These results suggested that the attained extracts are potential substitutes of synthetic antioxidants used in chemical, food and pharmaceutical industries.

Extração sortiva em barra de agitação para análise de fármacos em fluidos biológicos

A novel solventless sample preparation, stir-bar sorptive extraction (SBSE), for extraction, and sample enrichment of organic compounds from biological fluids, is described in this manuscript from principle to applications. The SBSE is based on sorptive extraction, whereby the compounds are extracted into a polymer coating, polydimethylsiloxane (PDMS), on a magnetic stirring rod. The extraction is controlled by the partitioning coefficient of drugs between the PDMS and sample matrix, and upon the sample-extraction medium phase ratio. The SBSE technique has been applied successfully, with high sensitivities, to biomedical analysis of volatiles and for semi-volatiles drugs from biological sample, including urine, plasma, and saliva. SBSE combined with in situ derivatization, drugs quite more polar (e.g. metabolites) also can be analyzed.

Aplicação da metodologia de superfície de resposta no estudo da produção e extração da poligalacturonase

The aim of this work was to verify the effects of initial medium moisture content (U), addition of ammonium sulphate (N) and of potassium phosphate (P) in the production of the polygalacturonase through the solid-state fermentation, using cashew apple husk as substrate and Aspergillus niger CCT0916 as transformation agent. We also studied the best extraction conditions of the produced enzyme. The best condition of production was with U of 40%, 1% of N and 0% of P being reached an activity of the poligalacturonase of 10.1 U/g. The best extraction condition is an agitation system with a time of 100 min and a solvent-fermented medium volume ratio of 5 mL/g.

Extração líquido-líquido de urânio(VI) do colofanito de itataia (Santa Quitéria, Ceará) por extratantes orgânicos em presença de ácido fosfórico

This work describes the liquid-liquid extraction of uranium after digestion of colofanite (a fluoroapatite) from Itataia with sulfuric acid. The experiments were run at room temperature in one stage. Among the solutions tested the highest distribution coefficient (D > 60) was found for 40%vol. DEHPA (di(2-ethyl-hexyl)phosphoric acid) + 20% vol. TOPO (trioctylphosphine oxide) in kerosene. Thorium in the raffinate was quantitatively extracted by TOPO (0.1% vol.) in cyclohexane. Uranium stripping and separation from iron was possible using 1.5 mol L-1 ammonium or sodium carbonate (room temperature, one stage). However, pH control is essential for a good separation.

Extração seletiva de metais pesados em sedimentos de fundo do Rio Tietê, São Paulo

Sediment samples from Tietê river were submitted to chemical and sequential extractions of heavy metals (Cd, Cr, Cu, Ni, Pb and Zn). It was followed a single extraction by using 0.1 mol L-1 hydrochloric acid and a sequential procedure to evaluate possible chemical associations described as exchangeable, carbonate, reducible oxides, sulfide, organic matter and residual fractions. High concentrations of heavy metals were determined at Pirapora reservoir, which is closer to the Metropolitan Area of São Paulo while for Barra Bonita reservoir, the results showed low concentrations for such elements. Acid volatile sulfides, grain size distribution and carbon contents were also determined.

Métodos de extração e qualidade da fração lipídica de matérias-primas de origem vegetal e animal

Methodologies of extraction of lipids from chicken breast and oats flakes were evaluated: Soxhlet, Folch et al., Bligh & Dyer and Hara & Radin. For chicken breast, the methods Soxhlet, Folch et al. and Bligh & Dyer presented the highest yields in total lipids. With oat flakes, the methods Soxhlet and Bligh & Dyer presented higher yields than the Hara & Radin and Folch et al. The Soxhlet method affected the quality of the lipid fraction in both samples. Extracted lipid components were separated by thin layer chromatography, the chloroform-methanol based was more efficient to extract the neutral and polar lipids.

Determinação de fósforo biodisponível em rações de peixes utilizando extração assistida por ultra-som e espectrofotometria no visível

The aim of the present work was to develop and optimize a method for determination of bioavailable phosphorus in samples of feces and fish feed using ultrasound extraction and subsequent quantification by visible spectrophotometry. Using as extractor solution HNO3 0.50 mol L-1, the great conditions of extraction established were: sample mass - 100 mg, samples granulometry - < 60 µm, sonification time - five cycles of 40 s and ultrasound potency - 136 W. The proposed method was applied in studies of digestibility of this nutrient in different feeds used in diets of juvenile of Nile tilapia.

Aplicação de planejamento fatorial a protocolo de extração e fixação de sulfetos volatilizáveis por acidificação (SVA) em amostras de sedimento

The AVS is defined operationally as acid volatile sulfide, which is a controlling phase on the partition of some metallic species in sediments. A Factorial design was evaluated by means of 16 experiments and using four variables: temperature, extraction time, N2 flow, and volume of the S2- collection solution. The factors that contributed to the efficiency of the process were the extraction time and the N2 flow. Trapping of S2- was efficient in AAB. The S2- was quantified using a potentiometric procedure. Recovery tests for S2- concentrations varying from 1&#215;10-5 to 1&#215;10-4 mol L-1 were in the range from 93 to 116%.

Extração e purificação de fármacos anti-inflamatórios não esteroidais ciclo-oxigenase-2 seletivos

Celecoxib (CB) and lumiracoxib (LM) are potent COX-2 inhibitors widely marketed for the treatment of rheumatoid arthritis and osteoarthritis. Nevertheless, it is difficult to obtain because it are protected under patents. The aim of this work was to develop an extraction method of drugs, CB and LM, in order to obtain the drug with a purity degree appropriated for use in research projects. The developed method showed to be effective of both drugs, becoming interesting due to its low cost, easy and speed of execution, application to different dosage forms (capsules and tablets) and drugs with different physicochemical properties.

Extração e purificação de clorofila a, da alga Spirulina maxima: um experimento para os cursos de química

This work describes a simple and economical experiment for the extraction and purification of chlorophyll a from Spirulina maxima. Extraction and purification of natural compounds can be considered one of the most illustrative experiments that can be performed in Organic Chemistry courses. Particularly, the chromatography of dyes and pigments allows students to have a better comprehension of the chromatography separations. These compounds represent an important class of organic pigments applied in pharmaceutical, cosmetic, detergent compositions, and various other fields and can be extracted from plants and algae. To extract, separate and purify chlorophyll a from associated pigments such as xanthophylls, carotenes, and pheophytins, very costly processes are reported. The present approach is perfectly adequate for use in Chemistry experiments for undergraduate students.

Estudo por espectroscopia micro-Raman dos mecanismos de separação de fase em vidros fosfatos de metais de transição

Glass-ceramics are prepared by controlled separation of crystal phases in glasses, leading to uniform and dense grain structures. On the other hand, chemical leaching of soluble crystal phases yields porous glass-ceramics with important applications. Here, glass/ceramic interfaces of niobo-, vanado- and titano-phosphate glasses were studied by micro-Raman spectroscopy, whose spatial resolution revealed the multiphase structures. Phase-separation mechanisms were also determined by this technique, revealing that interface composition remained unchanged as the crystallization front advanced for niobo- and vanadophosphate glasses (interface-controlled crystallization). For titanophosphate glasses, phase composition changed continuously with time up to the equilibrium composition, indicating a spinodal-type phase separation.