An analytical methodology based on coprecipitation-assisted coacervative extraction coupled to HPLC-UV was developed for determination of five organophosphorus pesticides (OPPs), including fenitrothion, guthion, parathion, methidathion, and chlorpyrifos, in water samples. It involves a green technique leading to an efficient and simple analytical methodology suitable for high-throughput analysis. Relevant physicochemical variables were studied and optimized on the analytical response of each OPP. Under optimized conditions, the resulting methodology was as follows: an aliquot of 9 mL of water sample was placed into a centrifuge tube and 0.5 mL sodium citrate 0.1 M, pH 4; 0.08 mL Al (SO ) 0.1 M; and 0.7 mL SDS 0.1 M were added and homogenized. After centrifugation the supernatant was discarded. A 700 μL aliquot of the coacervate-rich phase obtained was dissolved with 300 μL of methanol and 20 μL of the resulting solution was analyzed by HPLC-UV. The resulting LODs ranged within 0.7-2.5 ng/mL and the achieved RSD and recovery values were <8% (n = 3) and >81%, respectively. The proposed analytical methodology was successfully applied for the analysis of five OPPs in water samples for human consumption of different locations of Mendoza.
In the current context of climate change and water deficit, the selection of native beneficial microorganisms, such as plant growth‐promoting rhizobacteria (PGPR), has become a trend for sustainable agriculture due to their ability to improve plant–bacteria interaction with a minimal adverse effect on the soil microbiota compared to commercial PGPR. Until now, the production of phytohormones like melatonin (MT) by native PGPR and their effect on endogenous MT levels in plants have been poorly studied. MT is a ubiquitous phytohormone that protects plants against biotic and abiotic stress by improving the tolerance of stressed plants. In this work, the production of MT by two native PGPR, Enterobacter 64S1 and Pseudomonas 42P4, was evaluated and both PGPR were applied in Arabidopsis thaliana plants grown under drought conditions to assess the inoculation effects. Parameters such as plant growth, leaf cellular membrane damage, leaf protective compounds, and endogenous MT levels under drought and irrigation conditions were evaluated. The results demonstrated that the native strains Pseudomonas 42P4 and Enterobacter 64S1 produce MT and increase the content of endogenous MT in A. thaliana plants under drought. These native strains improved the tolerance of arabidopsis plants to drought by preventing oxidative and membrane damages and improving plant growth. To the best of our knowledge, this is the first report on MT production by native PGPR and their effects on endogenous MT levels in arabidopsis plants, setting the bases to elucidate the role of native PGPR on water deficit conditions.
Ultrasound-assisted extraction (UAE), cloud point extraction (CPE), and ultrasound back-extraction (UABE) techniques have been coupled for lixiviation, preconcentration, and cleanup of polybrominated diphenyl ethers (PBDEs) from milk samples for determination by gas chromatography-electron capture detection (GC-ECD). Physicochemical parameters that affect the efficiency of the extraction system were investigated using a design of experiments based on multivariate statistical tools, and considering the sample matrix along the development. The coupling of the leaching step, UAE, enhanced ca. 3.5 times the extraction efficiency of the former sample preparation methodology (CPE-UABE) leading to cleaner sample extracts suitable for GC analysis. Under optimum conditions, the proposed methodology exhibits successful performance in terms of linearity and precision, with recoveries in the range of 68-70% and LODs within the range 0.05-0.5 ng/g dry weight (d.w.). The proposed sample preparation methodology coupled three green analytical techniques. It expands the application frontiers of CPE for the analysis of biological samples by GC. The optimized methodology was used for determination of PBDEs in powder milk samples, from both commercial and human sources.
Enzymatic digestion, coupled to surfactant assisted‐dispersive liquid‐liquid microextraction (ED‐SA‐DLLME), is proposed as a mild innovative sample preparation methodology to determine polybrominated diphenyl ethers (PBDEs) in human hair samples by gas chromatography. The sodium dodecyl sulfate as a promoting agent in the ED stage also acts as a dispersive agent in DLLME, providing an advantageous synergy between sample preparation stages. Experimental variables of the ED‐SA‐DLLME were optimized using a multivariate method. The optimal experimental conditions were: proteinase K 0.96 U mL−1, SDS 1% (w/v), 37 °C, and 60 min for ED; and 50 μL tetrachloroethylene for SA‐DLLME. The notable analytical figures of merit showed LOQ in the range of 30–430 pg g−1, relative standard deviations <9%, and recoveries of 90–94%. The PBDEs were found in human hair samples <0.07 ng g−1.
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