Rapid detection and quantification of milk adulteration using infrared microspectroscopy and chemometrics analysis.

The application of attenuated total reflectance mid-infrared microspectroscopy (MIR-microspectroscopy) was evaluated as a rapid method for detection and quantification of milk adulteration. Milk samples were purchased from local grocery stores (Columbus, OH, USA) and spiked at different concentrations of whey, hydrogen peroxide, synthetic urine, urea and synthetic milk. Samples were place on a 192-well microarray slide, air-dried and spectra were collected by using MIR-microspectroscopy. Pattern recognition analysis by Soft Independent Modeling of Class Analogy (SIMCA) showed tight and well-separated clusters allowing discrimination of control samples from adulterated milk. Partial Least Squares Regression (PLSR) showed standard error of prediction (SEP) ~2.33, 0.06, 0.41, 0.30 and 0.014 g/L for estimation of levels of adulteration with whey, synthetic milk, synthetic urine, urea and hydrogen peroxide, respectively. Results showed that MIR-microspectroscopy can provide an alternative methodology to the dairy industry for screening potential fraudulent practice for economic adulteration of cow's milk.

Evaluation of the mineral profile of textile materials using inductively coupled plasma optical emission spectrometry and chemometrics.

The content of Al, Ba, Ca, Cr, Cu, Fe, Ni, P, Zn, Cd and Pb was determined in textile material samples after microwave-assisted decomposition in a cavity oven and extraction with an artificial sweat solution. Radial viewing inductively coupled plasma optical emission spectrometry (ICP OES) was the main detection technique, but Cd and Pb were determined by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to increase the sensitivity. Principal components analysis (PCA) was applied to the data sets to characterize the samples with respect to their geographic origin and color difference. The PCA for Brazilian single-color samples showed separation, with one group consisting of blue and green textiles and another with all the other materials evaluated. The geographic origin study showed a clear separation between Brazilian and Chinese textiles. The metals amount extracted with sweat extractable solution were lower than limits values pointed by the International Testing and Certification System for Textiles, Oko Tex Standard 100, in the all considered classes. Recoveries varied from 85 to 112% for additions ranging from 3.0 to 25 mg kg(-1) for Ca and from 0.3 to 7.0 mg kg(-1) for all other analytes through the microwave-assisted decomposition procedure.

Nutritional deficiency in citrus with symptoms of citrus variegated chlorosis disease.

It is well known that citrus plants that have been infected by Xylella fastidiosa display nutritional deficiencies, probably caused by production of extracellular polymers by the bacteria that block normal nutrient flow through the xylem. The aim of this work was to study the mineral composition of specific foliar areas in different stages of infection in citrus. Thus, the concentrations of macro and micronutrients in leaves of citrus infected by X. fastidiosa were measured. Samples from four infected citrus orchards in the State of São Paulo, Brazil, were respectively collected from Santa Rita do Passa Quatro, Neves Paulista, Gavião Peixoto and Paraíso counties. The presence of X. fastidiosa in leaves was confirmed by polymerase chain reaction (PCR) using specific PCR primers. To understand the variation in leaf-nutrient content in citrus plants, we used foliar nutrient values from control (non-symptomatic) plants as a reference. Chemometric analysis showed that the deficiency of P and K in symptomatic trees for all orchards and high concentrations of Fe, Mn and Zn were observed in chlorotic areas, although other studies revealed deficiency of zinc in leaves. This is the first report showing that a correlation between chlorotic citrus leaf and higher concentrations of Fe, Mn and Zn are observed when infected and healthy plants were compared.

Nutritional deficiency in citrus with symptoms of citrus variegated chlorosis disease / Deficiência nutricional em citros com sintomas da doença da clorose variegada dos citros

It is well known that citrus plants that have been infected by Xylella fastidiosa display nutritional deficiencies, probably caused by production of extracellular polymers by the bacteria that block normal nutrient flow through the xylem. The aim of this work was to study the mineral composition of specific foliar areas in different stages of infection in citrus. Thus, the concentrations of macro and micronutrients in leaves of citrus infected by X. fastidiosa were measured. Samples from four infected citrus orchards in the State of São Paulo, Brazil, were respectively collected from Santa Rita do Passa Quatro, Neves Paulista, Gavião Peixoto and Paraíso counties. The presence of X. fastidiosa in leaves was confirmed by polymerase chain reaction (PCR) using specific PCR primers. To understand the variation in leaf-nutrient content in citrus plants, we used foliar nutrient values from control (non-symptomatic) plants as a reference. Chemometric analysis showed that the deficiency of P and K in symptomatic trees for all orchards and high concentrations of Fe, Mn and Zn were observed in chlorotic areas, although other studies revealed deficiency of zinc in leaves. This is the first report showing that a correlation between chlorotic citrus leaf and higher concentrations of Fe, Mn and Zn are observed when infected and healthy plants were compared.

Já é bem conhecido que cultivares cítricas que foram infectadas pela bactéria Xylella fastidiosa apresentam deficiências nutricionais devido à produção de polímero extracelular por esta bactéria, o qual bloqueia o fluxo normal de nutriente pelo xilema. O objetivo deste trabalho foi o de estudar a composição mineral em áreas foliares específicas em diferentes fases de infecção na planta. Assim, as concentrações de macro e micronutrientes em folhas de citros infectados por X. fastidiosa foram quantificadas. Foram coletadas amostras de quatro pomares cítricos infectados localizados em: Santa Rita do Passa Quatro, Neves Paulista, Gavião Peixoto e Paraíso, no Estado de São Paulo. A presença de X. fastidiosa em folhas foi confirmada através de reação da polimerase em cadeia (PCR) usando iniciadores específicos. Para entender a variação no conteúdo de nutriente foliar em plantas cítricas, utilizou-se de valores de nutrientes foliares de plantas não sintomáticas (controle) como referência. A análise quimiométrica mostrou que a deficiência de P e K em plantas sintomáticas e concentrações altas de Fe, Mn e Zn foram presentes em áreas foliares cloróticas, embora outros estudos mostrem a deficiência de zinco em folhas. Este é o primeiro relato indicando que uma correlação entre folhas cítricas cloróticas e elevadas concentrações de Fe, Mn e Zn foi observada quando plantas infectadas e saudáveis foram comparadas.

Mechanised flow system for on-line microwave digestion of food samples with off-line catalytic spectrophotometric determination of cobalt at ng l-1 levels.

A mechanised system for on-line slurry food sample digestion was developed and an off-line cobalt determination was performed. The stabilised slurry sample was introduced into an air carrier stream until reaching the digestion coils located inside a household microwave oven. Software written in Visual Basic 3.0 was developed to permit the transport of the slurry samples and the programming of the microwave oven and also the control of the mineralization valve. The proposed system was optimized for determination of cobalt in certified samples such as mussels, bovine liver and fish and also uncertified fish samples. The digestion parameters were established as 3 mol l-1 HNO3 for mussels, 3 mol l-1 HNO3 plus 0.16% v/v H2O2 for bovine liver and 12 mol l-1 HNO3 for fish employing maximum power for 5 min of microwave actuation. In the subsequent spectrophotometric method for the catalytic determination of cobalt, the Tiron and hydrogen peroxide concentrations were 1.8 x 10(-3) and 3.0 x 10(-4) mol l-1, respectively, and the sample residence time was 300 s as determined by an optimisation process. The proposed method features a linear range from 10 to 200 ng l-1 Co (r > 0.996) with detection and quantification limits of 1.7 and 5.5 ng l-1 Co, respectively. The precision, expressed as RSD, was 2.4% (n = 12) for repeatability and 5.2% (n = 10) for reproducibility and the accuracy of the proposed method was assessed by using certified samples and an alternative technique (ETAAS).