Luis Antonio Minim

A green and sensitive method to determine phenols in water and wastewater samples using an aqueous two-phase system

A greener and more sensitive spectrophotometric procedure has been developed for the determination of phenol and o-cresol that exploits an aqueous two-phase system (ATPS) using a liquid-liquid extraction technique. An ATPS is formed mostly by water and does not require organic solvent. Other ATPS components used in this study were the polymer, polyethylene oxide, and some salts (i.e., Li(2)SO(4), Na(2)SO(4) or K(2)HPO(4)+KOH). The method is based on the reaction between phenol, sodium nitroprusside (NPS) and hydroxylamine hydrochloride (HL) in an alkaline medium (pH 12.0), producing the complex anion [Fe(2)(CN)(10)](10-) that spontaneously concentrates in the top phase of the system. The linear range was 1.50-500microgkg(-1) (R>or=0.9997; n=8) with coefficients of variation equal to 0.38% for phenol and 0.30% for o-cresol (n=5). The method yielded limits of detection (LODs) of 1.27 and 1.88microgkg(-1) and limits of quantification (LOQs) of 4.22 and 6.28microgkg(-1) for phenol and o-cresol, respectively. Recoveries between 95.7% and 107% were obtained for the determination of phenol in natural water and wastewater samples. In addition, excellent agreement was observed between this new ATPS method and the standard 4-aminoantipyrine (4-AAP) method.

PEO-[M(CN)5NO](x-) (M = Fe, Mn, or Cr) interaction as a driving force in the partitioning of the pentacyanonitrosylmetallate anion in ATPS: strong effect of the central atom.

The partitioning behavior of pentacyanonitrosilmetallate complexes[Fe(CN) 5 NO] (2-), [Mn(CN) 5 NO] 3(-), and [Cr(CN) 5 NO] 3(-)has been studied in aqueous two-phase systems (ATPS) formed by adding poly(ethylene oxide) (PEO; 4000 g mol (-1)) to an aqueous salt solution (Li2 SO4, Na2 SO4, CuSO4, or ZnSO4). The complexes partition coefficients ( K complex) in each of these ATPS have been determined as a function of increasing tie-line length (TLL) and temperature. Unlike the partition behavior of most ions, [Fe(CN) 5 NO] 2(-) and [Mn(CN) 5 NO] 3(-) anions are concentrated in the polymer-rich phase with K values depending on the nature of the central atom as follows: K [Fe(C N) 5 NO] 2 - >> K [ Mn (CN 5 NO] 3 - > K [C r (C N) 5 NO ]3 - . The effect of ATPS salts in the complex partitioning behavior has also been verified following the order Li2 SO 4 > Na2 SO 4 > ZnSO4. Thermodynamic analysis revealed that the presence of anions in the polymer-rich phase is caused by an EO-[M(CN) 5 NO] ( x- ) (M = Fe, Mn, or Cr) enthalpic interaction. However, when this enthalpic interaction is weak, as in the case of the [Cr(CN) 5 NO]3(-) anion ( K [Cr(CN 5 NO] 3 - < 1), entropic driving forces dominate the transfer process, then causing the anions to concentrate in the salt-rich phase.

Application of the response surface methodology for optimization of whey protein partitioning in PEG/phosphate aqueous two-phase system.

In order to develop a new strategy for β-lactoglobulin (β-lg) removal from whey protein, partitioning of α-lactalbumin (α-la), β-lg and glycomacropeptide (Gmp) was studied using aqueous two phase systems (ATPS). A system composed of 13% (w/w) polyethylene glycol (PEG, average molar mass 2000 g/mol) and 13% (w/w) potassium phosphate was used at 25°C. A central composite rotatable design (CCRD) associated to the response surface methodology (RSM) was applied to investigate the effects of NaCl concentration and pH on the partition of these proteins. It was found that α-la and Gmp partitioned to the top phase rich in PEG, whereas β-lg partitioned to the bottom phase rich in salt. According to the RSM, optimal conditions for β-lg removal where found where pH was equal to 6.7 and salt concentration was 0.35 mol/L. Under these conditions, the partition coefficient K(α) was 0.48 and K(Gmp) was 0.92. On the other hand, the partition coefficient K(β) was only 0.01. In such conditions β-lg preferentially concentrates in the bottom phase, while the top phase exclusively contains the proteins α-la and Gmp. Fractionation of the proteins from fresh whey was performed in a three stage cross-flow extraction system. The extraction yield for β-lg in the bottom phase was 97.3%, while the yields for α-la and Gmp in the top phase were 81.1% and 97.8%, respectively.

Use of response surface methodology to evaluate the extraction of Debaryomyces hansenii xylose reductase by aqueous two-phase system

Xylose reductase (XR) from Debaryomyces hansenii was extracted by partitioning in aqueous two-phase systems (ATPS) composed of polyethylene glycol (PEG) 4000 in the presence of different salts, specifically sodium sulfate, lithium sulfate and potassium phosphate. Batch extractions were carried out under different conditions of temperature (25-45 degrees C) and tie-line length (TLL) for each system, according to a central composite design face-centered of 36 tests, and the response surface methodology was used to evaluate the results. Quadratic polynomial models were adjusted to the data to predict the behavior of four responses, namely the XR partition coefficient (K(XR)), the selectivity (S), the purification factor (PF(T)) and the activity yield (Y(T)) in the top phase. The optimal extraction conditions were found using the PEG 4000/sodium sulfate system at 45 degrees C and TLL=25.1, which ensured PF(T)=3.1 and Y(T)=131%. The ATPS proved effective for partial purification of D. hansenii xylose reductase in cell-free crude extract, and the response surface methodology revealed to be an appropriate and powerful tool to determine the best dominion of temperature and ATPS composition.

Rapid detection of whey in milk powder samples by spectrophotometric and multivariate calibration

A rapid method for the detection and quantification of the adulteration of milk powder by the addition of whey was assessed by measuring glycomacropeptide protein using mid-infrared spectroscopy (MIR). Fluid milk samples were dried and then spiked with different concentrations of GMP and whey. Calibration models were developed using multivariate techniques, from spectral data. For the principal component analysis and discriminant analysis, excellent percentages of correct classification were achieved in accordance with the increase in the proportion of whey samples. For partial least squares regression analysis, the correlation coefficient (r) and root mean square error of prediction (RMSEP) in the best model were 0.9885 and 1.17, respectively. The rapid analysis, low cost monitoring and high throughput number of samples tested per unit time indicate that MIR spectroscopy may hold potential as a rapid and reliable method for detecting milk powder frauds using cheese whey.

Sistema aquoso bifásico: uma alternativa eficiente para extração de íons

Solvent extraction has been successfully applied to metal ion preconcentration and often meant the use of toxic organic diluents. However, regulatory pressure is increasingly focusing on the use and disposal of organic solvents, and thus the development of nonhazardous alternatives is important. In this review, we examine the application of aqueous biphasic systems (ABS) to extraction of ions, analyzing their potential and limitations and suggest that ABSs could be an efficient substitute for oil/water biphasic systems. ABSs are formed by mixing certain inorganic salts and water-soluble polymers, or by mixing two water-soluble polymers.

Influence of the temperature and type of salt on the phase equilibrium of peg 1500 + potassium phosphate and peg 1500 + sodium citrate aqueous two-phase systems

The present work analyzed the effect of the temperature and type of salt on the phase equilibrium of aqueous two-phase systems (ATPS) formed by poly (ethylene glycol) (PEG) 1500 + potassium phosphate, from (278.15 to 318.15) K, and PEG 1500 + sodium citrate, from (278.15 to 298.15) K. The rise of the temperature normally increased the slope of the tie line (STL). With respect to the influence of the type of salt, sodium citrate showed better capability to induce phase separation, when compared to potassium phosphate.

Estudo de mercado de iogurte da cidade de Belo Horizonte/MG

O estudo do perfil dos consumidores e dos fatores envolvidos no processo de compra do iogurte e uma ferramenta importante na identificacao dos diferentes segmentos desse mercado e de suas potencialidades. Assim, neste trabalho entrevistaram-se 387 consumidores de iogurte, residentes em Belo Horizonte - MG, que responderam os questionarios estruturados. Os resultados foram analisados de forma descritiva, e para verificar a correlacao entre caracteristicas sociodemograficas com o perfil de consumo aplicou-se a analise de correlacao de Pearson. Os resultados indicaram que o iogurte sabor morango apresenta maior aceitacao pelos consumidores, que a categoria light/diet possui grande parte do seu publico consumidor (54%). Segundo a pesquisa, 39,9% dos respondentes que nao consomem iogurte light/diet disseram nao consumi-lo por nao gostar desse produto. Isto revela a importância de pesquisas para desenvolvimento de iogurte light/diet visando a melhoria da qualidade sensorial. O fato de nao ver necessidade de consumir o produto foi apontado como um dos principais motivos por nao consumir iogurte da categoria light/diet. A qualidade, a marca e o preco apresentaram grande importância na conquista de mercado, sendo os tres principais atributos observados no momento da compra de iogurte na cidade estudada. Analisando a correlacao entre consumo e fator sociodemografico, observou-se que a renda e a idade influenciam tanto na frequencia de consumo de iogurte quanto no consumo do produto na versao light/diet.

Development and validation of the high performance liquid chromatography-ion exclusion method for detection of lactic acid in milk

The present work reports the development and validation of an analytical method for lactic acid quantification in milk by ion exclusion-HPLC with UV detection. This method showed good precision (variation coefficient <7.0%) and good accuracy (97.6-99.6%). Calibration curves were linear (R(2)>0.996) at the tested range of 5.0-25.0mmolL(-1); and the detection and quantification limits were 0.5 and 1.0mmolL(-1), respectively. Analysis of lactic acid in fermented milk (FM) or NaOH neutralised fermented milk (FNM) was performed using samples obtained during 9h of fermentation. An ANOVA analysis combined with the Tukey test was used to show that the method was insensitive to the differences between FM and FNM. The proposed method therefore proved to be a useful quality control tool in laboratories because it was able to determine milk acidity even in adulterated samples.

Modeling Thermal Conductivity, Specific Heat, and Density of Milk: A Neural Network Approach

Abstract The accurate determination of thermophysical properties of milk is very important for design, simulation, optimization, and control of food processing such as evaporation, heat exchanging, spray drying, and so forth. Generally, polynomial methods are used for prediction of these properties based on empirical correlation to experimental data. Artificial neural networks are better suited for processing noisy and extensive knowledge indexing. This article proposed the application of neural networks for prediction of specific heat, thermal conductivity, and density of milk with temperature ranged from 2.0 to 71.0°C, 72.0 to 92.0% of water content (w/w), and 1.350 to 7.822% of fat content (w/w). Artificial neural networks presented a better prediction capability of specific heat, thermal conductivity, and density of milk than polynomial modeling. It showed a reasonable alternative to empirical modeling for thermophysical properties of foods.