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The absence of gluten proteins in sorghum allows for the production of baked goods that are suitable for celiacs. Previous studies have shown that the milling process affects the performance of sorghum flour in baked products, especially those that are gluten-free (GF). This study aimed to explore the effects of mill type (impact and roller) on flour properties and GF bread quality by assessing the technological quality, antioxidant activity, and mineral content of the bread. All particle populations of flour obtained via both millings presented a bimodal distribution, and the volume mean diameter (D 4,3) ranged from 431.6 µm to 561.6 µm. The partially refined milled flour obtained via polishing and impact milling produced bread with a soft crumb, fewer but larger alveoli in the crumb, and a structure that did not collapse during baking, showing the best performance in bread quality. In the in vitro bread digestibility assay, the total polyphenol content and antioxidant activity decreased during the digestion steps. High mineral (Cu, Fe, Mn, and Zn) contents were also found in a portion of the bread (120 g) made with whole sorghum flour; however, their potential bioavailability was reduced in the presence of a higher amount of bran.

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Food products, especially those with high value-added, are commonly subjected to strict quality controls, which are of paramount importance, especially for attesting to some peculiar features related, for instance, to their geographical origin and/or the know-how of their producers. However, the sophistication of fraudulent practices requires a continuous update of analytical platforms. Different analytical techniques have become extremely appealing since the instrumental analysis tools evolution has substantially improved the capability to reveal and understand the complexity of food. In light of this, multi-elemental composition has been successful implemented solving a plethora of food authentication and traceability issues. In the last decades, it has existed an ever-increasing trend in analysis based on spectrometry analytical platforms in order to obtain a multi-elemental profile that combined with chemometrics have been noteworthy analytical methodologies able to solve these problems. This review provides an overview of published reports in the last decade (from 2011 to 2021) on food authentication and quality control from their multi-element composition in order to evaluate the state-of-the-art of this field and to identify the main characteristics of applied analytical techniques and chemometric data treatments that have permit achieve accurate discrimination/classification models, highlighting the strengths and the weaknesses of these methodologies.

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Sorghum is the fourth most important cereal produced in Argentina and the fifth worldwide. It has good agronomic characteristics and could be developed in arid areas, allowing a wide geographic distribution. Its starch content, higher than 70%, makes it possible to obtain a good yield of flours. Nutritionally, it should be noted that the grain does not have the protein fraction called prolamins, which makes it suitable for consumption by people with celiac disease. The multielemental composition constitutes an important indicator of the nutritional profile of the grains and allows, together with other parameters, to select the most suitable varieties for human consumption. In its determination, the preanalytical stage is decisive to obtain a reliable result. Organic samples are a challenge for sample introduction systems that use plasma-based techniques. As an alternative to conventional pretreatment with a microwave-assisted digestion (MWAD), a greener, quick, and simple treatment is proposed, using ultrasound-assisted extraction (UAE) in diluted acid media. The UAE method accelerates analysis times, improves performance and productivity, and was applied to sorghum samples cultivated in the province of La Pampa (Argentina). Microwave-induced plasma optical emission spectrometry (MIP OES) was employed for the determination of Cu, K, Mg, Mn, P, and Zn. The detection limits found ranged from 0.6 (Cu) to 89 (P) mg kg-1, and the precision expressed by the relative standard deviation (RSD) was ≤7.7% (Zn). For validation, a maize reference material (NCS ZC 73010) was evaluated. The principal component analysis revealed three different groupings related to the sorghum varieties' mineral profile.

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Based on green analytical chemistry principles it is important to evolve procedures that convert solid samples into solutions without using excessive reagent quantities, energy, temperature, and avoiding waste generation. To reach this aim, a simple infrared assisted digestion (IRAD) method for animal feed analysis was proposed. Infrared radiation (IR) with 2 mL of HNO3 and 2 mL of H2O2 were assessed, presenting low dissolved organic carbon (DOC) and residual acidity (RA) in the final digest, being fully compatible with microwave induced plasma atomic emission spectrometry (MIP OES). Calcium, Cd, Cu, Fe, K, Mg, Na, P, Sr and Zn were determined in reference materials and in animal feeds. Limits of quantification were between 2.52 and 284 mg kg-1 for Ca and P respectively. Recovery values ranged 80-120%, with relative standard deviations (RSD%) under 8%. The friendliness offered by the IRAD MIP OES method was evaluated by two green indexes. Concentrations in feedstuffs were compared with National Research Council (NRC) recommendations.

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An overview about the presence of arsenic (As) in groundwaters of Argentina, made by a transdisciplinary group of experts is presented. In this second part, the conventional and emerging technologies for As removal, management of wastes, and the initial investment costs of the proposed technologies, with emphasis on developments of local groups are described. Successful examples of real application of conventional and emerging technologies for As removal in waters for human consumption, for medium, small and rural and periurban communities are reported. In the country, the two most applied technologies for arsenic removal at a real scale are reverse osmosis and coagulation-adsorption-filtration processes using iron or aluminum salts or polyelectrolytes as coagulants. A decision tree to evaluate the possible technologies to be applied, based on the population size, the quality of the water and its intended use, is presented, including preliminary and indicative investment costs. Finally, a section discussing the treatment and final disposal of the liquid, semiliquid and solid wastes, generated by the application of the most used technologies, is included. Conclusions and recommendations, especially for isolated rural and periurban regions, have been added.

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An overview about the presence of arsenic (As) in groundwaters of Argentina, made by a transdisciplinary group of experts is presented. Aspects on As occurrence, effects of As on human health, regulations regarding the maximum allowable amount of As in drinking water as well as bottled water, and analytical techniques for As determination are presented. The most affected region in Argentina is the Chaco-Pampean plain, covering around 10 million km2, where approximately 88% of 86 groundwater samples collected in 2007 exceeded the World Health Organization (WHO) guideline value. In the Salí river basin, As concentrations ranged from 11.4 to 1660 µg/L, with 100% of the samples above the WHO guideline value. In the Argentine Altiplano (Puna) and Subandean valleys, 61% of 62 samples collected from surface and groundwaters exceeded the WHO limit. Thus, it can be estimated that, at present, the population at risk in Argentina reaches around four million people. Pathologies derived from the chronic consumption of As, the metabolism of As in the human body and the effects of the different As chemical forms, gathered under the name HACRE (hidroarsenicismo crónico regional endémico in Spanish, for chronic regional endemic hydroarsenicism) are described. Regarding the regulations, the 10 µg/L limit recommended by the WHO and the United States Environmental Protection Agency has been incorporated in the Argentine Food Code, but the application is still on hold. In addition, there is disparity regarding the maximal admitted values in several provinces. Considerations about the As concentrations in bottled water are also presented. A survey indicates that there are several Argentine laboratories with the suitable equipment for As determination at 10 µg/L, although 66% of them are concentrated in Buenos Aires City, and in the Santa Fe, Córdoba and Buenos Aires provinces. Conclusions and recommendations of this first part are provided.

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The capacity of Elodea canadensis to phytofiltrate arsenic species from water was evaluated. Plants were adapted to tap water and supplemented with 15 and 250 µg L-1 of As. Inorganic arsenic species (As III, As V), and organic arsenic compounds: monomethylarsonate (MMA) and dimethylarsinate (DMA) were analyzed. Sampling was carried out at different times after exposure in culture water and plant organs. Plants exposed to 15 µg L-1 of As concentration showed no significant difference on As concentration (95% confidence level) in their organs compared to controls. When plants were exposed to 250 µg L-1 of As concentration, a significant increase of As concentration in plant organs was observed. After 1 h exposure, plants reduce 63.16% the As concentration in the culture water, with a bioaccumulation factor (BF) of 4.3. Under these conditions, E. canadensis accumulate As V in roots and do not translocate it to stems (transfer factor <1). MMA was determined in stems and leaves. E. canadensis effectively phytofiltrate As from tap water of a city located in an arsenic endemic area from concentrations of 36 µg L-1 to undetectable levels (10 ng L-1).

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A straightforward and rapid single-tube sample pretreatment for wear metals determination in used lubricating oils was developed in this work as an alternative to the reference pretreatment method (ASTM). A D-optimal mixture design on a three-component solution was performed. The optimal composition for the proposed sample preparation emulsion was 2% v/v of xylene, 9.5% v/v of Triton®X-114% and 88.5% v/v of H2O. The determination of 18 wear metals was carried out by microwave induced plasma with optical emission spectrometer (MIP OES), and the results of the two sample preparations -conventional and proposed- were statistically compared. Also, a certified standard "wear metals in used lubricating oils" for pretreatment validation was used. The developed method was as effective as the reference method indicated by ATSM, similar in speed and simplicity, but superior from the environmental and economic point of view. The proposed pretreatment allowed Ag, Al, Ba, Ca, Cd, Cr, Cu, K, Mg, Mn, Mo, Ni, Pb, Si, Sn, Ti, V and Zn determination, with LOQ between 1.40 mg kg-1 for Ca and 6.34 mg kg-1 for Pb. The precisions established as the relative standard deviation (RSD) were better than 6.2%. The proposed method avoid sample handling, reducing contamination risks and analyte losses, affording significantly improvement on wear metal quantification.

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Arthrospira platensis and Arthrospira maxima are a type of blue-green microalga used as a dietary supplement (Spirulina). A low time-consuming ultrasound-assisted digestion (UAD) of Spirulina supplements for multielemental determination by microwave induced plasma atomic emission spectrometry (MPAES) was performed. Several parameters such as acid concentration (AC), thermostated water bath (TWB), digestion time (DT) and UAD - probe or bath - affecting the digestion process were evaluated through a full factorial design. Under the optimal conditions -100 °C for TWB, 5% for AC and 10 min for DT- and selecting the bath as the proper UAD system, the concentrations of 15 analytes (Al, Ba, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, V, Zn) were reported. The values are in accordance with the recommendation established by Food and Drug Administration (FDA) excepting for Cd. The knowledge of Spirulina multielemental composition contributes to an outstanding nutritional and toxicological report for human health.

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A single-step procedure for trace elements analysis of milk samples is presented. Solubilization with small amounts of dymethylformamide (DMF) was assayed prior to inductively coupled plasma mass spectrometry (ICPMS) detection with a high efficiency sample introduction system. All main instrumental conditions were optimized in order to readily introduce the samples without matrix elimination. In order to assess and mitigate matrix effects in the determination of As, Cd, Co, Cu, Eu, Ga, Gd, Ge, Mn, Mo, Nb, Nd, Ni, Pb, Pr, Rb, Sm, S, Sr, Ta, Tb, V, Zn, and Zr, matrix matching calibration with (103)Rh as internal standard (IS) was performed. The obtained limits of detection were between 0.68 (Tb) and 30 (Zn) µg L(-1). For accuracy verification, certified Skim milk powder reference material (BCR 063R) was employed. The developed method was applied to trace elements analysis of commercially available milks. Principal components analysis was used to correlate the content of trace metals with the kind of milk, obtaining a classification according to adults, baby or baby fortified milks. The outcomes highlight a simple and fast approach that could be trustworthy for routine analysis, quality control and traceability of milks.

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Trace metals have negative effects on the oxidative stability of edible oils and they are important because of possibility for oils characterisation. A single-step procedure for trace elemental analysis of edible oils is presented. To this aim, a solubilisation with tetramethylammonium hydroxide (TMAH) was assayed prior to inductively coupled plasma mass spectrometry detection. Small amounts of TMAH were used, resulting in high elemental concentrations. This method was applied to edible oils commercially available in Argentine. Elements present in small amounts (Cu, Ge, Mn, Mo, Ni, Sb, Sr, Ti, and V) were determined in olive, corn, almond and sunflower oils. The limits of detection were between 0.004 µg g(-1) for Mn and Sr, and 0.32 µg g(-1) for Sb. Principal components analysis was used to correlate the content of trace metals with the type of oils. The two first principal components retained 91.6% of the variability of the system. This is a relatively simple and safe procedure, and could be an attractive alternative for quality control, traceability and routine analysis of edible oils.

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A study about the capabilities of three kinds of nanomaterials namely, carbon nanotubes (CNT), oxidized carbon nanotubes (ox-CNT) and l-alanine immobilized on carbon nanotubes (ala-CNT) to serve as sorbents for preconcentrating Ni and Pb using an on-line system coupled to electrothermal atomic absorption spectroscopy (ETAAS) technique, was accomplished. The solid phase extraction was performed in a conical minicolumn used as sorbent holder. After loading a fixed volume of the analytes, they were eluted with a discrete volume (50 µL) of nitric acid, placed directly into the platform of a L'Vov tube. After that, each analyte was determined individually. Ni and Pb retention was strongly influenced by pH but exhibiting different behaviors. The study demonstrated that the sorbent based on ox-CNTs was the one that exhibited the highest capacity and linearity for both analytes when compared with CNT or ala-CNT. The analytical performance was evaluated for the three sorbents to establish the best conditions regarding sensitivity, reproducibility and accuracy. The precision expressed as relative standard deviations (n=6) were 3.9 and 0.5% for Ni(2+) and Pb(2+), respectively The limit of detection (LOD), calculated as the concentration required to yield a net peak equal to three times the standard deviation of the background signal (3σ) was 30 and 10 ng L(-1) for Ni(2+) and Pb(2+) respectively. Alternatively, the limit of quantification (10σ) was calculated and resulted to be 0.79 and 0.07 µg L(-1) for Ni(2+) and Pb(2+) respectively. After optimization, the method that involved the use of ox-CNT associated to an on-line preconcentration was tested in samples of relevant environmental importance. Accuracy was evaluated analyzing a certified reference material namely, Municipal Sludge (QC MUNICIPAL SLUDGE A) and a reference sample of Lake Sediment (TRAP-LRM from IJS).

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An interference-free, fast, and simple method is proposed for Pb determination in environmental solid samples combining slurry sampling and electrothermal atomic absorption spectrometry. Samples were ground to an adequate particle size and slurries were prepared by weighing from 0.05 g to 0.20 g of dry sediment, adding nitric acid, and a solution containing 0.1% Triton X-100. Ultrasonic agitation was employed for slurries homogenization. Analytical variables including acid pre-treatment conditions, particle size, slurry stability, temperature program of the graphite furnace, and type and concentration of the chemical modifier were studied. The undesirable effects of potential non-specific and spectral interferences on Pb signal were also taken into account. Continuum source and self-reversal methods for background correction were evaluated and compared. For calibration, synthetic acid solutions of Pb were employed. Calibration was linear within the range 1-30 microg L(-1) and 5-30 microg L(-1) when the 217.0 nm and 283.3 nm analytical lines were used. Correlation coefficients of 0.9992 and 0.9997 were obtained. Using optimized conditions, limits of detection (3sigma) of 0.025 microg g(-1) and 0.1 microg g(-1) were achieved for the 217.0 nm and 283.3 nm analytical lines, respectively. The method was successfully applied to the determination of lead in soil, contaminated soil, municipal sludge, and sediment samples. The accuracy was assessed by the analysis of two certified reference materials: municipal sludge (QC MUNICIPAL SLUDGE A) and lake sediment (TRAP-LRM from IJS).

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