Determination and Evaluation of Metallothionein and Metals in Mugil cephalus (Mullet) from Pontal Bay, Brazil.

To assess environmental contamination, studies have been increasingly carried out using biomarkers to diagnose the effects of toxic metal exposure, such as metallothionein (MT). In this context, the aims of the present study were to determine Cd, Cu, Ni and Pb concentrations, by ICP-MS, in liver samples from Mugil cephalus from the municipality of Ilhéus, located in North-Southeastern Brazil, in the state of Bahia, which has been increasingly suffering from anthropogenic pressure, and to quantify total MT in liver and gills. Among essential metals, copper (199.2 µg g-1) presented concentrations approximately 7 times higher than allowed by the World Health Organization (30 µg g-1). Liver samples showed higher concentrations than gills. Metallothionein concentrations indicate differential contamination along the study area. The first sampling showed higher induction of MT synthesis overall. Differences between liver and gill MT concentration trends were relatively minor, which may indicate the adequacy of analyzing gills in an environmental monitoring context.

A new and accessible instrumentation to determine urea in UHT milk using digital image analysis.

This research demonstrates the development, optimization and application of a new low-cost detection system, based on digital image analysis, for the detection of urea in ultra-high-temperature (UHT) milk samples. The apparatus built in the laboratory, allows the capture of images through a simple system built by polyvinyl chloride (PVC) tubes, a digital microscope and a peristaltic mini-pump, after the colorimetric reaction between urea and diacetylmonoxime (butane-2,3-dionammonoxime). The red, green and blue (RGB) and hue, saturation and value (HSV) color systems were studied, with the saturation channel of the HSV color system selected as the analytical signal. Subsequently, the experimental chemical conditions were evaluated through multivariate experimental designs and the optimal conditions were defined. The proposed method was validated, and the detection and quantification limits presented by the method were 0.35 mg L-1 and 0.52 mg L-1, respectively; precision, ranged between 1.6  and 2.8 %. The results were compared with those obtained using the mid-infrared technique and no statistically significant differences were observed at a 95 % confidence level. The proposed method was applied to eight UHT milk samples that presented urea content ranging from 187 to 386 mg L-1. The mean values obtained are in agreement with values presented in other studies for the determination of urea in milk. The results indicated that the system described and validated here is promising and can be applied to assess the authenticity and quality of milk.

Homogeneity and stability assessment of a candidate to pumpkin seed flour reference material by means of computer vision based chemometrics assisted approach.

This study proposes a preliminary assessment of the homogeneity and stability through digital image acquisition of a candidate for mechanically processed pumpkin seed meal reference material, exploring the concepts of homogeneity curve and the analysis of texture characteristics by Continuous-Level Moving Block through Robust Principal Component Analysis. This innovative methodology allowed us to examine the percentage of homogeneity in a set of samples, revealing an average of 41% with only one outlier in relation to the entire sample, indicating low homogeneity. In the stability study carried out after storing samples for 12 months at different temperatures, 83% of the samples were considered regular and 17% were outlier, which means that most of them were considered stable. Therefore, this methodology is useful for screening samples for homogeneity, by textural analysis, and detected non-homogeneity can be corrected in advance for quantification by standard protocols.

Characterization of the chemical composition (mineral, lead and centesimal) in pine nut (Araucaria angustifolia (Bertol.) Kuntze) using exploratory data analysis.

In this study, mineral composition, centesimal composition and lead were evaluated in pine nut seeds (raw and cooked) from five Brazilian states. Mineral composition was determined by ICP OES and lead by GF AAS. The results for minerals were evaluated by Boxplot, PCA and HCA, using the R software. Average minerals in raw and cooked samples (mg 100 g-1) were: 15.2 and 10.8 (Ca), 0.168 and 0.113 (Cu), 0.506 and 0.330 (Fe), 536 and 420 (K), 51.3 and 40.6 (Mg), 0.373 and 0.208 (Mn), 132 and 102 (P) and 0.746 and 0.520 (Zn). The average centesimal composition (raw and cooked) was: 53.5 and 47.2% (moisture), 1.76 and 1.26% (ash), 3.90 and 3.53% (protein), 40.8 and 48.0% (carbohydrate) and 179 and 206 kcal/100 g (total caloric value) and Pb was not detected. The chemometric analysis showed a distinction of raw and cooked samples due to significant nutrient losses after thermal processing.

Simultaneous optimization of multiple responses and its application in Analytical Chemistry - A review.

This manuscript covers the application of the main techniques for simultaneous optimization of multiple responses generated by the application of multivariate designs (two-factor factorial, Central Composite, Doehlert, etc.) or by chromatographic runs in the development of analytical methods. Special attention will be given to the graphical method, desirability function, multiple response function and chromatographic response functions, since they are more frequently used in the analytical area. The advantages, disadvantages, limitations, and potentialities of these methods will also be addressed, as well as some of their applications, commenting on real examples from the literature. Some less usual methods in multiple response optimization in Analytical Chemistry will also be commented.

Screening of Mangifera indica L. functional content using PCA and neural networks (ANN).

A method using reversed-phase high-performance liquid chromatography with diode array detection (HPLC-DAD) was applied after extraction with acidified methanol, to determine 12 bioactive phenolic compounds in the peel and pulp of the mango fruit (Mangifera indica L.) cultivated in the Bahia, state of Brazil. The proposed methodology was previously fully validated and proven successful in the analysis of methanolic extracts of lyophilized samples. The limits of quantification ranged between 0.78 and 3.14 mg L-1 and the individual recovery values obtained for the spiked samples ranged from 80% to 120%. The results were evaluated using PCA and ANN. The results indicate that the fruits are rich in polyphenols, mainly: ellagic acid, gallic acid, rutin and catechin, which contribute to their greater use as functional foods, natural antioxidants and in the pharmaceutical industry, as well as other applications.

Homogeneity study of a corn flour laboratory reference material candidate for inorganic analysis.

In this work, a homogeneity study of a corn flour reference material candidate for inorganic analysis is presented. Seven kilograms of corn flour were used to prepare the material, which was distributed among 100 bottles. The elements Ca, K, Mg, P, Zn, Cu, Fe, Mn and Mo were quantified by inductively coupled plasma optical emission spectrometry (ICP OES) after acid digestion procedure. The method accuracy was confirmed by analyzing the rice flour certified reference material, NIST 1568a. All results were evaluated by analysis of variance (ANOVA) and principal component analysis (PCA). In the study, a sample mass of 400mg was established as the minimum mass required for analysis, according to the PCA. The between-bottle test was performed by analyzing 9 bottles of the material. Subsamples of a single bottle were analyzed for the within-bottle test. No significant differences were observed for the results obtained through the application of both statistical methods. This fact demonstrates that the material is homogeneous for use as a laboratory reference material.

Determination and evaluation of the metals and metalloids in the Chapeu-de-couro (Echinodorus macrophyllus (Kunth) Micheli).

The Chapeu-de-couro (Echinodorus macrophyllus (Kunth) Micheli) is a native plant from Brazil, which has been mainly used in medicinal application being a potent antirheumatic and diuretic, in the production of soft drinks, and also in the ornamentation of aquariums. In this paper, the metals and metalloids for the leaves of chapeu-de-couro collected in the Paraguacu River from the city Cachoeira, Bahia State, Brazil, was determined and evaluated using multivariate analysis. The samples were digested using nitric acid and hydrogen peroxide and were analyzed using inductively coupled plasma mass spectrometry. The accuracy of the method was confirmed by analysis of a certified reference material of apple leaves, furnished by National Institute of Standard and Technology. The study involved 15 samples of the Paraguacu River. The results expressed as milligrams of element per kilogram of sample demonstrated that the concentration ranges varied: 1.39-5.27 for chromium, 44.85-165.39 for manganese, 0.55-0.84 for arsenic, 0.01-3.94 for antimony, and 0.18-0.31 for lead. The principal component analysis and hierarchical cluster analysis evidenced that the concentrations of the metals and metalloids varied according with the variations in the water of the Paraguacu.