Tungsten coil atomic emission spectrometry combined with dispersive liquid–liquid microextraction: A synergistic association for chromium determination in water samples

A novel and environment friendly analytical method is reported for total chromium determination and chromium speciation in water samples, whereby tungsten coil atomic emission spectrometry (WCAES) is combined with in situ ionic liquid formation dispersive liquid–liquid microextraction (in situ IL-DLLME). A two stage multivariate optimization approach has been developed employing a Plackett–Burman design for screening and selection of the significant factor involved in the in situ IL-DLLME procedure, which was later optimized by means of a circumscribed central composite design. The optimum conditions were complexant concentration: 0.5% (or 0.1%); complexant type: DDTC; IL anion: View the MathML sourcePF6−; [Hmim][Cl] IL amount: 60 mg; ionic strength: 0% NaCl; pH: 5 (or 2); centrifugation time: 10 min; and centrifugation speed: 1000 rpm. Under the optimized experimental conditions the method was evaluated and proper linearity was obtained with a correlation coefficient of 0.991 (5 calibration standards). Limits of detection and quantification for both chromium species were 3 and 10 µg L−1, respectively. This is a 233-fold improvement when compared with chromium determination by WCAES without using preconcentration. The repeatability of the proposed method was evaluated at two different spiking levels (10 and 50 µg L−1) obtaining coefficients of variation of 11.4% and 3.6% (n=3), respectively. A certified reference material (SRM-1643e NIST) was analyzed in order to determine the accuracy of the method for total chromium determination and 112.3% and 2.5 µg L−1 were the recovery (trueness) and standard deviation values, respectively. Tap, bottled mineral and natural mineral water samples were analyzed at 60 µg L−1 spiking level of total Cr content at two Cr(VI)/Cr(III) ratios, and relative recovery values ranged between 88% and 112% showing that the matrix has a negligible effect. To our knowledge, this is the first time that combines in situ IL-DLLME and WCAES.The authors would like to thank the Spanish Ministry of Science and Innovation (Project no. CTQ2011-23968), Spanish Ministry of Education, Culture and Sport (Project no. PHB2010-0018-PC), Generalitat Valenciana (Spain) (Project no. ACOMP/2013/072), and Coordenação de Aperfeiçoamento de Pessoal de Nível Superior in Brazil (Grant CAPES-DGU n. 243/11). L. Vidal also thanks the Spanish Ministry of Education, Culture and Sport for her travel Grant (HBP-2010-0030) and S.G. Silva is grateful to the Grant 2011/13288-7, São Paulo Research Foundation (FAPESP)

Optimizing a sustainable ultrasound assisted extraction method for the recovery of polyphenols from lemon by-products:comparison with hot water and organic solvent extractions

Response surface methodology (RSM) based on a three-factor and three-level Box–Behnken design was employed for optimizing the aqueous ultrasound-assisted extraction (AUAE) conditions, including extraction time (35–45 min), extraction temperature (45–55 °C) and ultrasonic power (150–250 W), for the recovery of total phenolic content (TPC) and rutin from lemon by-products. The independent variables and their values were selected on the basis of preliminary experiments, where the effects of five extraction parameters (particle size, extraction time and temperature, ultrasonic power and sample-to-solvent ratio) on TPC and rutin extraction yields were investigated. The yields of TPC and rutin were studied using a second-order polynomial equation. The optimum AUAE conditions for TPC were extraction time of 45 min, extraction temperature of 50 °C and ultrasonic power of 250 W with a predicted value of 18.10 ± 0.24 mg GAE/g dw, while the optimum AUAE conditions for rutin were extraction time of 35 min, extraction temperature of 48 °C and ultrasonic power of 150W with a predicted value of 3.20 ± 0.12 mg/g dw. The extracts obtained at the optimum AUAE conditions were compared with those obtained by a hot water and an organic solvent conventional extraction in terms of TPC, total flavonoid content (TF) and antioxidant capacity. The extracts obtained by AUAE had the same TPC, TF and ferric reducing antioxidant power as those achieved by organic solvent conventional extraction. However, hot water extraction led to extracts with the highest flavonoid content and antioxidant capacity. Scanning electron microscopy analysis showed that all the extraction methods led to cell damage to varying extents

The Application of Zeta Potential for the Effective Retention of Titanium Dioxide in Chemically Modified Systems

This study was done to determine how to obtain maximum effective filler retention in a fiber and titanium dioxide system. Retention of fillers in a fibrous system is greatly influenced through the use of high molecular weight polymers. It was found that by using cationic and anionic polymers in the same system, a synergistic effect results which yields a higher effective retention than if either polymers were used along. Furthermore, by precisely controlling the amounts of each polymer so as to obtain the isoelectric point in zeta potential; the peak effective retention is reached

The Use of Cationic Agents to Increase the Efficiency of Titanium Dioxide in Paper

Handsheets were made with a bleached sulfite pulp, titanium dioxide and cationic agents. The optical properties of these sheets were studied in order to determine and compare the efficiency of the titanium dioxide retained. The cationic agents used in this study were a quaternary ammonium salt, a polyamide, cationic starches made with these two chemicals, and a commercial cationic starch. When the optical properties of handsheets made from these substances were compared, it was found that the quaternary ammonium salt gave the highest opacity but the lowest retention. The polyamide gave lower opacities but higher retentions. The cationic starches made from these cationic chemicals showed slightly lower opacities than the cationic chemicals by themselves but they gave much higher retentions. The commercial cationic starch gave intermediate retention but lower opacity. It was concluded that the quaternary ammonium salt gave the best dispersion of the titanium dioxide but gave the lowest cationic charge to the pigment. The polymide gave a slightly poorer dispersion but gave a much higher charge to the pigment. The cationic starches gave the best retention through a combination of mechanical and physio-chemical retention, but did not disperse the pigment too well

Metabolomics : a tool for studying plant biology

In recent years new technologies have allowed gene expression, protein and metabolite profiles in different tissues and developmental stages to be monitored. This is an emerging field in plant science and is applied to diverse plant systems in order to elucidate the regulation of growth and development. The goal in plant metabolomics is to analyze, identify and quantify all low molecular weight molecules of plant organisms. The plant metabolites are extracted and analyzed using various sensitive analytical techniques, usually mass spectrometry (MS) in combination with chromatography. In order to compare the metabolome of different plants in a high through-put manner, a number of biological, analytical and data processing steps have to be performed. In the work underlying this thesis we developed a fast and robust method for routine analysis of plant metabolite patterns using Gas Chromatography-Mass Spectrometry (GC/MS). The method was performed according to Design of Experiment (DOE) to investigate factors affecting the extraction and derivatization of the metabolites from leaves of the plant Arabidopsis thaliana. The outcome of metabolic analysis by GC/MS is a complex mixture of approximately 400 overlapping peaks. Resolving (deconvoluting) overlapping peaks is time-consuming, difficult to automate and additional processing is needed in order to compare samples. To avoid deconvolution being a major bottleneck in high through-put analyses we developed a new semi-automated strategy using hierarchical methods for processing GC/MS data that can be applied to all samples simultaneously. The two methods include base-line correction of the non-processed MS-data files, alignment, time-window determinations, Alternating Regression and multivariate analysis in order to detect metabolites that differ in relative concentrations between samples. The developed methodology was applied to study the effects of the plant hormone GA on the metabolome, with specific emphasis on auxin levels in Arabidopsis thaliana mutants defective in GA biosynthesis and signalling. A large series of plant samples was analysed and the resulting data were processed in less than one week with minimal labour; similar to the time required for the GC/MS analyses of the samples

Recent progress in mitochondria-targeted drug and drug-free agents for cancer therapy

The mitochondrion is a dynamic eukaryotic organelle that controls lethal and vital functions of the cell. Being a critical center of metabolic activities and involved in many diseases, mitochondria have been attracting attention as a potential target for therapeutics, especially for cancer treatment. Structural and functional differences between healthy and cancerous mitochondria, such as membrane potential, respiratory rate, energy production pathway, and gene mutations, could be employed for the design of selective targeting systems for cancer mitochondria. A number of mitochondria-targeting compounds, including mitochondria-directed conventional drugs, mitochondrial proteins/metabolism-inhibiting agents, and mitochondria-targeted photosensitizers, have been discussed. Recently, certain drug-free approaches have been introduced as an alternative to induce selective cancer mitochondria dysfunction, such as intramitochondrial aggregation, self-assembly, and biomineralization. In this review, we discuss the recent progress in mitochondria-targeted cancer therapy from the conventional approach of drug/cytotoxic agent conjugates to advanced drug-free approaches

2D-ReS2 & diamond nanoparticles-based sensor for the simultaneous determination of sunset yellow and tartrazine in a multiple-pulse amperometry FIA system

We present a flow injection system with a multiple pulse amperometric detection (FIA-MPA)-based methodology for the simultaneous analysis of sunset yellow and tartrazine. As transducer, we have developed a novel electrochemical sensor based on the synergistic effect of ReS2 nanosheets and diamond nanoparticles (DNPs). Among several transition dichalcogenides for the sensor development, we have selected ReS2 nanosheets since it yields a better response towards both colourants. Scanning probe microscopy characterization shows that the surface sensor is composed by scattered and stacked ReS2 flakes and large aggregates of DNPs. With this system, the gap between the oxidation potential values of sunset yellow and tartrazine is wide enough to allow the simultaneous determination of both dyes. Under the optimum potential pulse conditions (0.8 and 1.2 V) during 250 ms, a flow rate of 3 mL/min and a volume injection of 250 μL, detection limits of 3.51 × 10− 7 M and 2.39 × 10− 7 M for sunset yellow and tartrazine, respectively, were obtained. This method exhibits good accuracy and precision with Er minor than 13% and RSD lower than 8% with a sampling frequency of 66 samples per hour. Pineapple jelly samples were analyzed by the standard addition method, obtaining 53.7 mg/kg and 29.0 mg/kg of sunset yellow and tartrazine, respectively. From the analysis of fortified samples, recoveries of 94% and 105% were obtainedThe authors acknowledge financial support from projects PID2020- 113142RB-C21 and PID2020-113142RB-C22 and TED2021-129416 AI00 funded by MCIN/AEI/10.13039/501100011033 and P2018/NMT4349 (TRANSNANOAVANSENS-CM) funded by the Comunidad Autonoma ´ de Madrid. We thank L. Chico for fruitful discussion

Modelling the effect of combined antimicrobials: A base model for multiple-hurdles

Combining antimicrobials to reduce microbial growth and to combat the potential impact of antimicrobial resistance is an important subject both in foods and in pharmaceutics. Modelling of combined treatments designed to reduce or eliminate microbial contamination in foods (microbiological predictive modelling) has become commonplace. Two main reference models are used to analyse mixtures: the Bliss Independence and the Loewe reference models (LRM). By using optical density to analyse the growth of Aeromonas hydrophila, Cronobacter sakazakii and Escherichia coli in combined NaCl/NaCl (a mock combination experiment) and combined NaCl/KCl experiments, previous models for combined antimicrobials in foods, based on the Bliss approach, were shown to be inconsistent and that models based on the LRM more applicable. The LRM was shown, however, to be valid only in the specific cases where the concentration exponents of all components in a mixture were identical. This is assured for a mock combination experiment but not for a true mixture. This, essentially, invalidates the LRM as a general reference model. A new model, based on the LRM but allowing for mixed exponents, was used to analyse the combined inhibition data, and concluded that the NaCl/KCl system gave the additive effect expected from literature studies. This study suggests the need to revise current models used to analyse combined effects