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1.
Sci Total Environ ; 805: 150348, 2022 Jan 20.
Article in English | MEDLINE | ID: mdl-34818759

ABSTRACT

A new highly sensitive, selective, and inexpensive electrochemical method has been developed for simultaneously detecting diethylstilbestrol (DES) and 17ß-estradiol (E2) in environmental samples (groundwater and lake water) using a graphite sensor modified by cerium oxide nanoparticles (CPE-CeO2 NPs). The developed sensor and the materials used in its preparation were characterized using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD). The ab initio simulation was used to evaluate the adsorption energies between both DES and E2 with the surface of the sensor. The peak current of oxidation of both hormones showed two regions of linearity. The region of greatest sensitivity was observed for the linear range of 10 nM-100 nM. The detection and quantification limits for this concentration range were 0.8/2.6 nM and 1.3/4.3 nM for DES and E2, respectively. The analytical performance of the developed method showed high sensitivity, precision, repeatability, reproducibility, and selectivity. The CPE-CeO2 NPs sensor was successfully applied to simultaneously detect DES and E2 in real samples with recovery levels above 98%.


Subject(s)
Diethylstilbestrol , Electrochemical Techniques , Electrodes , Estradiol , Limit of Detection , Reproducibility of Results
2.
Sci Total Environ ; 749: 142385, 2020 Dec 20.
Article in English | MEDLINE | ID: mdl-33370922

ABSTRACT

Excessive and indiscriminate use of the herbicide glyphosate (GLY) leaves the environment susceptible to its contamination. This work describes the development of a simple, inexpensive, and efficient electroanalytical method using graphite oxide paste electrode (GrO-PE) for the direct determination of GLY traces in groundwater samples, soybean extracts, and lettuce extracts. Under optimal experimental conditions, the developed sensor exhibited a linear response of the peak current intensity vs. the concentration, in the range of 1.8 × 10-5 to 1.2 × 10-3 mol L-1 for GLY. The limits of detection and quantification are 1.7 × 10-8 mol L-1 and 5.6 × 10-8 mol L-1, respectively. The methodology developed here demonstrated a strong analytical performance, with high reproducibility, repeatability, and precision. Moreover, it successfully avoided interference from other substances, showing high selectivity. The GrO-PE sensor was effectively applied to determine GLY traces in real samples with recovery rates ranging from 98% to 102%. Results showed that the GrO-PE is effective and useful for GLY detection, with the advantage of not involving laborious modifications and complicated handling, making it a promising tool for environmental analysis.

3.
Mater Sci Eng C Mater Biol Appl ; 105: 110048, 2019 Dec.
Article in English | MEDLINE | ID: mdl-31546367

ABSTRACT

A simple, inexpensive, highly sensitive, selective, and novel electrochemical method was developed for determination of the Bisphenol A in samples of tap water, blood serum, and urine using a bentonite-modified carbon paste electrode. The graphite, bentonite and the working electrodes (without and chemically modified) were characterized by scanning electron microscopy, infrared absorption spectroscopy, and X-ray diffraction. The electrodes were electrochemically characterized using cyclic voltammetry, square wave voltammetry, and electrochemical impedance spectroscopy. The studied electrochemical variables were: electrode area, standard heterogeneous rate constant, charge transfer coefficient and double-layer capacitance. The bentonite as a sensor modifier had a strong influence on these variables. For the development of the methodology to quantify Bisphenol A, the instrumental parameters (frequency, amplitude, and step potential) and experimental parameters (pH, bentonite quantity) were optimized. The analytical curve to Bisphenol showed a linear response of the oxidation peak current intensity vs. the concentration in the range of 6.8 × 10-10 to 1.5 × 10-8 mol mL-1, with a limit of detection (LOD) of 2.11 × 10-11 mol mL-1 and limit of quantification (LOQ) of 7.04 × 10-11 mol mL-1. Recovery experiments were performed by adding known amounts of Bisphenol A in tap water, blood serum, and urine samples. Recovery rates using the standard addition method were in the range of 97.8-101.8%. The results demonstrated the method feasibility for quantifying Bisphenol A in these samples.


Subject(s)
Bentonite/chemistry , Benzhydryl Compounds/analysis , Electrochemical Techniques , Phenols/analysis , Electrodes , Graphite/chemistry , Limit of Detection , Oxidation-Reduction
4.
J Environ Sci Health B ; 53(12): 817-823, 2018.
Article in English | MEDLINE | ID: mdl-30325268

ABSTRACT

This paper describes a simple, inexpensive, highly sensitive, selective, and efficient electrochemical method to determine glyphosate (GLY) in samples of milk, orange juice, and agricultural formulation. The oxidation reaction on the electrode surface was electrochemically characterised by cyclic voltammetry (CV) and square wave voltammetry (SWV). The investigation of GLY at carbon paste electrode revealed a non-reversible oxidation peak at +0.95 V versus Ag/AgCl, which was used for electrochemical detection of GLY. The operating parameters (pH, frequency, step potential, and amplitude) were optimised in relation to the peak current intensity, and a calibration curve was set up in a concentration range of 4.40 × 10-8-2.80 × 10-6 mol L-1, with a detection limit of 2 × 10-9 mol L-1. After calibration curve was plotted, the developed procedure was applied to determine GLY in previously contaminated samples: milk and orange juice, and in a commercial formulation, obtaining recovery values between 98.31% and 103.75%. These results show that the proposed method can be used for GLY quantification in different samples with high sensitivity, specificity, stability, and reproducibility.


Subject(s)
Carbon/analysis , Electrodes , Fruit and Vegetable Juices/analysis , Glycine/analogs & derivatives , Milk/chemistry , Animals , Citrus sinensis , Electrochemical Techniques , Glycine/analysis , Hydrogen-Ion Concentration , Limit of Detection , Oxidation-Reduction , Reproducibility of Results , Sensitivity and Specificity , Glyphosate
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