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Here, lab-made graphite and polylactic acid (Gpt-PLA) biocomposite materials were used to additively manufacture electrodes via the fused deposition modeling (FDM) technique for subsequent determination of the explosive 2,4,6-trinitrotoluene (TNT, considered a persistent organic pollutant). The surface of the 3D-printed material was characterized by SEM and Raman, which revealed high roughness and the presence of defects in the graphite structure, which enhanced the electrochemical response of TNT. The 3D-printed Gpt-PLA electrode coupled to square wave voltammetry (SWV) showed suitable performance for fastly determining the explosive residues (around 7 s). Two reduction processes at around -0.22 V and -0.36 V were selected for TNT detection, with linear ranges between 1.0 and 10.0 µM. Moreover, detection limits of 0.52 and 0.66 µM were achieved for both reduction steps. The proposed method was applied to determine TNT in different environmental water samples (tap water, river water, and seawater) without a dilution step (direct analysis). Recovery values between 98 and 106% confirmed the accuracy of the analyses. Additionally, adequate selectivity was achieved even in the presence of other explosives commonly used by military agencies, metallic ions commonly found in water, and also some electroactive camouflage species. Such results indicate that the proposed device is promising to quantify TNT residues in environmental samples, a viable on-site analysis strategy.

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In this work, a vortex-assisted dispersive liquid-liquid microextraction method, using an ionic liquid as the extracting solvent was developed, for the simultaneous analysis of three UV filters in different water samples. The extracting and dispersive solvents were selected in a univariate way. Then, the parameters such as the volume of the extracting and dispersive solvents, pH and ionic strength were evaluated using a full experimental design 24, followed by Doehlert matrix. The optimized method consisted of 50 µL of extracting solvent (1-octyl-3-methylimidazolium hexafluorophosphate), 700 µL of dispersive solvent (acetonitrile) and pH of 4.5. When combined with high-performance liquid chromatography, the method limit of detection ranged from 0.3 to 0.6 µg L-1, enrichment factors between 81 and 101%, and the relative standard deviation between 5.8 and 10.0%. The developed method demonstrated effectiveness in concentrating UV filters in both river and seawater samples, being a simple and efficient option for this type of analysis.

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Fluoroquinolones (FQs) are broad-spectrum antibiotics widely used to treat animal and human infections. The use of FQs in these activities has increased the presence of antibiotics in wastewater and food, triggering antimicrobial resistance, which has severe consequences for human health. The detection of antibiotics residues in water and food samples has attracted much attention. Herein, we report the development of a highly sensitive online solid-phase extraction methodology based on a selective molecularly imprinted polymer (MIP) and fluorescent detection (HPLC-FLD) for the determination of FQs in water at low ng L−1 level concentration. Under the optimal conditions, good linearity was obtained ranging from 0.7 to 666 ng L−1 for 7 FQs, achieving limits of detection (LOD) in the low ng L−1 level and excellent precision. Recoveries ranged between 54 and 118% (RSD < 17%) for all the FQs tested. The method was applied to determining FQs in river water. These results demonstrated that the developed method is highly sensitive and selective.

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A simple, sensitive and reproducible solid-phase extraction method using plastic cartridges containing a monolithic sorbent (m-SPE), coupled to reverse phase liquid chromatography analysis, aiming to determine fifteen polycyclic aromatic hydrocarbons in surface water samples, was developed. The sorbent was easily prepared through a thermal polymerization reaction by using a mixture of n-butyl methacrylate as non-polar monomer and ethylene glycol dimethacrylate as crosslinker contained in a typical Polypropylene syringe cartridge. The effect of different parameters (type of hydrophobic monomer, elution solvent, sample volume, sorbent amount and sorbent load capacity) on the extraction efficiency was optimized. The optimal conditions were achieved by using n-butyl methacrylate as monomer, tetrahydrofurane (THF) as solvent for sorbent cleaning, THF:acetone (1:1) as elution solvent, 25.00 mL of sample volume, 600 µL of the polymerization mixture and 60 µg L-1 as sample loading capacity. Finally, the sorbent charge capacity, the reusability of the cartridges and the extraction efficiency of the m-SPE monolith, as compared with a typical C8 cartridge, were evaluated. Under the optimized experimental conditions, enrichment factors were between 76 and 103, relative recovery factors from 78 to 103%, accuracy values in the range of 58 to 98%, and inter-batch reproducibility values from between 2 and 10%, were obtained. The limits of detection and quantification were obtained by two different procedures: the signal to noise (S/N) ratios (3 and 10, respectively) and the IUPAC convention. The lowest LOD and LOQ values, obtained with the S/N ratios, were between 0.02 and 1.00 µg L-1, respectively whereas with the IUPAC convention the values were between 0.07 and 5 µg L-1. Using this procedure, several PAHs could be detected in the surface water sample taken from a river stream located in La Plata city (Buenos Aires Province, Argentina).

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The following work presents the development of the solid phase extraction technique with rotary disk (RDSE) in which the analysis for seven triazines in surface waters was first implemented. All the variables involved in extraction have been studied and optimized using a solid phase of octadecyl (C18) deposited on surface of the disk. Triazines were analyzed quantitatively by gas chromatography with simple quadruple mass detector, recoveries obtained for seven triazines were between 80% and 120%, accuracy expressed as RSD was between 3.21% and 6.34%, and detection limit of the method was between 0.020-0.056 µgL-1 according to each analyte, which indicates a good reproducibility and precision of the method. Finally, the method was applied to analyze the objective compounds in water samples obtained in the Bolo River (Palmira-Colombia), in which triazines were not detected.

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In this work, nanoporous gold (NPG) was prepared according to three different approaches, such as (i) anodization-electrochemical reduction (A-ECR, NPGA), (ii) dynamic hydrogen bubble template (DHBT, NPGB), and (iii) the combination of both methods (NPGA+B). Field-emission scanning electron microscopy (FE-SEM) and cyclic voltammetry (CV) were used to investigate the structural morphology and the electrochemical behavior of the fabricated materials. The NPGA+B electrode showed a large amount of surface defects and/or edges, greater electrochemical surface area (2.5 cm2), and increased roughness factor (35.4). Such outstanding features of the NPGA+B platform were demonstrated by the sensitive detection of methyl parathion (MP) in river water samples. CV results indicated nearly 25-fold, 6-fold, and 2.5-fold higher sensitivity for NPGA+B compared to that of bare Au, NPGA, and NPGB, respectively. Differential pulse voltammetry (DPV) results show a linear behavior in the MP concentration range of 5-50 ng mL-1 with a limit of detection (LOD) of 0.6 ng mL-1 and limit of quantification (LOQ) of 2.0 ng mL-1. Besides, the NPGA+B sensor also revealed excellent selectivity towards MP detection in the presence of other interfering molecules or ions, reproducibility, and repeatability.

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The hollow fiber liquid-phase microextraction allows highly selective concentration of organic compounds that are at trace levels. The determination of those analytes through the supercritical fluid chromatography usage is associated with many analytical benefits, which are significantly increased when it is coupled to a mass spectrometry detector, thus providing an extremely sensitive analytical technique with minimal consumption of organic solvents. On account of this, a hollow fiber liquid-phase microextraction technique in two-phase mode combined with supercritical fluid chromatography coupled to mass spectrometry was developed for quantifying 19 multiclass emerging contaminants in water samples in a total chromatographic time of 5.5 min. The analytical method used 40 µL of 1-octanol placed in the porous-walled polypropylene fiber as the acceptor phase, and 1 L of water sample was the donor phase. After extraction and quantification techniques were optimized in detail, a good determination coefficient (r2 > 0.9905) in the range of 0.1 to 100 µg L-1, for most of the analytes, and an enrichment factor in the range of 7 to 28,985 were obtained. The recovery percentage (%R) and intraday precision (%RSD) were in the range of 80.80-123.40%, and from 0.48 to 16.89%, respectively. Limit of detection and quantification ranged from 1.90 to 35.66 ng L-1, and from 3.41 to 62.11 ng L-1, respectively. Finally, the developed method was successfully used for the determination of the 19 multiclass emerging contaminants in superficial and wastewater samples.

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A dispersive micro-solid phase extraction (d-µ-SPE) procedure was developed for the simultaneous extraction of 39 multiclass pesticides, containing a variety of chemical groups (organophosphate, organochlorine, pyrethroid, strobilurin, thiocarbamate, triazole, imidazole, and triazine), from water samples. A customized d-µ-SPE glass device was combined with a multi-tube platform vortex and a micro-desorption unit (Whatman Mini-UniPrep G2 syringeless filter), which allowed the unique simultaneous desorption, extract filtration, and injection. A simplex-centroid mixture design and Doehlert design were employed to optimize the extraction conditions. The optimized extraction conditions consisted of an extraction time of 30 min, an addition of 6.74 % of NaCl into 100 mL of water sample, and a desorption time of 24 min with 500 µL of EtAc. The procedure provided a low limit of detection (LOD), ranging from 0.51 ng L-1 (4,4-DDE) to 22.4 ng L-1 (dimethoate), and an enrichment factor ranging from 72.5 (dimethoate) to 200 (tebuconazole). The relative recoveries of the pesticides from spiked freshwater and seawater ranged from 74.2 % (endrin) to 123 % (molinate). The proposed procedure was applied to detect the presence of multiclass pesticides in environmental water samples. Three pesticides commonly applied in Brazil, namely, malathion, dimethoate, and lambda-cyhalothrin, were detected in concentrations ranging from

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A água utilizada em serviços de hemodiálise passa por um sistema de tratamento a fim de garantir que os parâmetros microbiológicos e físico-químicos estejam adequados e proporcionem segurança ao paciente. Este trabalho avaliou a qualidade da água antes e após esta passar por sistema de tratamento em dois serviços (A e B) de hemodiálise em Santarém. Foram coletadas amostras de água em três pontos: Ponto 1 (P1) após saída do poço, Ponto 2 (P2) na saída do tratamento e Ponto 3 (P3) na máquina de hemodiálise. Testes microbiológicos e físico-químicos foram realizados e os resultados mostraram que não houve crescimento de coliformes totais e Escherichia coli nas amostras. No serviço A, houve contaminação por bactérias heterotróficas em 87% das amostras, destas, 27% ocorreram no P3. O pH mostrou-se menor que 6,0 no P1 nos dois serviços, normalizando os seus valores no P3. No serviço A, concentrações superiores ao recomendado de alumínio e nitrato foram verificadas em 100% das amostras coletadas no P1, os valores foram normalizados na saída do tratamento (P2). A pesquisa demonstrou que, para os parâmetros estudados, a qualidade da água, após passar por sistema de tratamento, é satisfatória, com exceção das bactérias heterotróficas no serviço A. (AU)

The water used in hemodialysis services goes through a treatment system in order to ensure that the microbiological and physicochemical parameters are adequate and provide safety to the patient. This work evaluated the quality of water before and after it went through a treatment system in two hemodialysis services (A and B) in Santarém. Water samples were collected at three points: Point 1 (P1) after leaving the well, Point 2 (P2) leaving the treatment and Point 3 (P3) on the hemodialysis machine. Microbiological and physical-chemical tests were performed and the results showed no growth of total coliforms and Escherichia coli in the samples. In service A, there was contamination by heterotrophic bacteria in 87% of the samples, 27% of which occurred in P3. The pH was less than 6.0 in P1 in both services, normalizing its values in P3. Service A, concentrations higher than the recommended amount of aluminum and nitrate were verified in 100% of the samples collected in P1, the values were normalized at the end of the treatment (P2). The research demonstrated that, for the studied parameters, the water quality, after going through a treatment system, is satisfactory, with the exception of heterotrophic bacteria in service A. (AU)

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Rapid, on-site detection of emerging pollutants is critical for monitoring health threats and the environment, especially if performed through autonomous systems. In this paper, we report on a new design of a complete electrochemical system whose working (WE), auxiliary (AE) and reference (RE) electrodes were obtained on a pen (PEN Sensor) made with graphite:polyurethane (GPUE). Working electrodes were decorated with spherical, ca. 200 nm silver nanoparticles (AgNPs) reduced on graphite using the polyol method. Differential pulse voltammetry (DPV) was used to detect bisphenol-A (BPA) in a linear range from 2.5 to 15 µmol L-1 with detection limit of 0.24 µmol L-1. The PEN Sensor could also detect bisphenol-A in tap and river water samples, with satisfactory reproducibility and repeatability, while common interferents did not affect electrooxidation of bisphenol-A. The high sensitivity and rapid detection are suitable for real-time analysis and in loco monitoring of emerging pollutants. With their robustness and versatility, PEN Sensors such as those fabricated here may be integrated into futuristic smart robotic systems.

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A molecularly imprinted polymer was synthesized and characterized to be used as solid-phase extraction sorbent for simultaneous chlorpyrifos and diazinon and their oxon derivatives. Several imprinted polymers were prepared and evaluated in a retention study of these analytes compared with a non-printed polymer. Several parameters affecting the extraction of imprinted polymer such as washing solvent, composition and volume of the eluting solvent and sample volume, were also investigated. Under the optimum conditions, the developed method provided satisfactory limits of detection ranging between 0.07 µg L-1 to 0.12 µg L-1 and the material showed an excellent reusability (> 50 reuses). The method was applied to the extraction and preconcentration of these analytes in water samples. The average recoveries ranged from 79 ± 6 to 104 ± 3 %.

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An analytical methodology has been developed and validated for the purpose of identifying and quantifying four parabens (methylparaben, ethylparaben, propylparaben and n-butylparaben) in water samples. The combination of rotating disk sorptive extraction (RDSE) technology with ultra-high performance liquid chromatography (UHPLC), along with electrospray ionization source (ESI) and time of flight mass spectrometry (TOF/MS) in trap mode, allowed for eliminating derivatization processes and a reduction of the chromatographic time required, achieving a greener analytical method. In this method, detection limits and precision (%RSD) were lower than 0.018 µg L-1 and lower than 9.7% for all the parabens, respectively, being better than similar works. Matrix effect and absolute recoveries were studied in tap and sewage water samples to observe suppressions of the signals for all analytes, and absolute recoveries were around 60%. This methodology was applied to the analysis of two sewage samples (punctual and composite) obtained from locations in Santiago, Chile.

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Nonsteroidal anti-inflammatory agents (NSAIDs) are a group of pharmaceuticals considered one of the most popular drugs used in clinical practice applied to the treatment of acute and chronic conditions. Some pharmaceuticals products are excreted reaching the environment and altering the balance of ecosystems. This work proposes a new fluorimetric flow injection (FI) methodology for the NSAID tolfenamic acid quantification based on the quenching effect of the analyte on fluorescent signal of bovine serum albumin fluorophore. Results put in evidence a mechanism of static quenching, with a Stern Volmer constant value of 1.8 × 107 L mol-1. To achieve the selective on-line preconcentration of analyte, a carbon nanotubes mini column was introduced in the FI configuration producing a beneficial effect on high sampling frequency, minimum sample and reagents consumption. The experimental factors that influence batch fluorescent signal and FI analysis have been studied and optimized. At optimal experimental conditions, an adequate tolerance to foreign species was shown. With the flow configuration, a LOD of 0.019 µg L-1, a LOQ of 0.058 µg L-1 were obtained with a sampling rate of 30 samples h-1. The new methodology was successfully applied to analyte determination in tap water and pharmaceutical and factory waste samples with recuperation near to 100%.

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In this study, a high throughput approach to rotating-disk sorptive extraction (RDSE) using laminar cork as extraction phase is demonstrated for the first time in the determination of 20 multiclass organic micro-pollutants including pesticides, PAHs and UV filters compounds from aqueous samples with gas chromatography mass spectrometry (GC-MS). The influencing parameters (desorption solvent, volume and time, extraction time and sample pH and ionic strength) were carefully optimized using multivariate designs. The optimal conditions were 10 min for extraction using 35 mL of water samples and a liquid desorption using 1 mL of MeOH:AcOEt (50:50% v/v) for 20 min. A low-cost apparatus that allows six extractions simultaneously, providing a high throughput of 5 min per sample turnaround times, considering the sample preparation step was used for the first time in this modified RDSE methodology. Satisfactory analytical performance was achieved with limits of detection (LOD) between 0.08 and 1.5 µg L-1 and limits of quantification (LOQ) between 0.3 and 4.8 µg L-1. The relative recoveries for the analytes were determined using river and lake water samples spiked at different concentrations and ranging from 80% to 119% for all analytes, with relative standard deviations (RSD) lower than 20%. The extraction efficiency obtained for the proposed configuration with laminar cork was significantly superior to powdered cork, demonstrating an interesting new configuration for new applications.

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This paper describes a new configuration of the hollow fiber renewal liquid membrane (HFRLM) procedure for the high-throughput determination of the endocrine disrupting compounds 4-nonylphenol, 4-octylphenol, 4-tert-octylphenol, methylparaben, ethylparaben and bisphenol A using a 96-well plate system and high-performance liquid chromatography. In this configuration, cylindrical blades were adapted as a support for polypropylene membranes used as supported liquid membranes in the HFRLM approach. The proposed configuration exhibited important advantages including high-throughput, low solvent and sample consumption, and good analytical performance. The optimized extraction conditions were achieved with the use of a mixture comprised of 50:50 v/v 1-octanol:hexane as the supported liquid membrane, sample pH 5, extraction solvent 15 µL (hexane) and extraction time 45 min. The limits of quantification varied from 0.5 µg L-1 for 4-octylphenol to 15 µg L-1 for methylparaben and ethylparaben and the r2 ranged from 0.9908 for methylparaben to 0.9992 for 4-tert-octylphenol. HFRLM combined with the use of a 96-well plate provides an environmentally-friendly configuration. It offers good accuracy when applied to analyze water samples, with relative recoveries ranging from 72 to 130%, for 4-octylphenol and 4-nonylphenol, respectively, and precision varying from 1 to 14.3%, for 4-nonylphenol at 1.0 µg L-1 and bisphenol A at 8.0 µg L-1, respectively.

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This work proposes the quantification of Cr (VI) ions in natural waters in trace level, using activated alumina (Al2O3) as preconcentration support, controlled in-line dissolution of the solidified chromophore diphenylcarbazide after heat treatment and spectrophotometric detection. The manifold ensures high sensitivity of analytical response, good repeatability, and stability. In this work, optimization of experimental conditions of a flow injection system was chosen as the parameters for greater sensitivity and better selectivity. The selected optimized conditions were 0.30 mol L-1 for H2SO4 concentration, system flow rate as 0.40 mL min-1, sample injection volume of 192.50 µL, 2 min for preconcentration time, and 0.10 mol L-1 for eluent concentration. The analytical curves obtained for real sample analysis show linear range from 0.192 to 0.961 µM, linear correlation coefficient R = 0.9997 and LOD = 0.024 µM. The preconcentration factor of about four times was obtained through the passage of 800 µL of a standard solution containing 0.961 µM of Cr (VI) through mini-column of preconcentration followed by elution at 192.5 µL of NH4OH 0.1 mol L-1 solution. The solid chromogenic reagent presented high durability (weeks in daily use with mass of 0.0993 g) and good reproducibility in analytical signal. The reactivation of the mini-column of alumina should be executed after ten injections of eluent, using 800 µL of HCl 0.02 mol L-1 solution in flow through the same. Each cycle of injection and elution of the sample takes about 5 min on the proposed terms. Despite the length of each cycle still be high, low concentrations can be detected using a technique of relatively low cost. This is due in part, the association dissolution of the chromogenic reagent directly in the line and the preconcentration step. Another important factor is the economy of reagent chromogenic, low generation of reject contributing to better quality of the environment, and the high potential for applications to work in field.

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The polished silver solid amalgam electrode (p-AgSAE) combined with square wave voltammetry (SWV) was used in the development of an analytical procedure to Methomyl determination in natural water samples. The experimental and voltammetric parameters were optimized and the use of cationic surfactant cetyltrimethyl ammonium bromide promoted a considerable change in the kinetic and mechanism of the Methomyl reaction. Was observed the presence one-single reduction peak, related to a totally irreversible two-electrons transfer, followed by chemical reaction involving two protons. Analytical parameters (linearity range, analytical curve equations, correlation coefficient, detection and quantification limits, recovery efficiency, and relative standard deviation for intraday and interday experiments) were evaluated indicating that the proposed voltammetric procedure is suitable for determination of Methomyl. The application of the proposed procedure in natural water analysis indicated high robustness with only simple filtration, without pre-concentration steps, good stability and suitable sensitivity to determination of Methomyl in natural water samples.

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A monolithic column affording complexing groups was synthesized for automated solid-phase extraction of potentially toxic metal ions in a low-pressure sequential injection analyzer. Poly(glycidyl methacrylate-co-ethylene dimethacrylate) monoliths were synthesized by free-radical polymerization in the coffins of fused silica-lined stainless-steel tubes (2.10 mm i.d. × 5-6 cm length). High permeability (4.33 × 10-13 m2) was achieved for monoliths polymerized for 24 h at 60 °C from a mixture of 30 wt% glycidyl methacrylate, 10 wt% ethylene glycol dimethacrylate, 35 wt% n-propanol, 20 wt% 1,4 butanediol and 5 wt% water. Azobisisobutyronitrile (1 wt% with respect to the monomers) initiated the free-radical polymerization. These generic columns were modified with iminodiacetate to create complexing functionalities on the polymer surface, being further used for online solid-phase extraction of Cu2+, Pb2+ and Cd2+ from natural, tap and drinking waters prior to their determination by stripping chronopotentiometry. The high permeability of the column allowed the loading, washing, eluting and reconditioning steps to be made at flow rate of 10 µL s-1. The limits of detection and quantification achieved by processing 1500 µL of sample were 0.51 and 1.7 µg L-1 for Cu2+, 1.4 and 4.7 µg L-1 for Pb2+, and 1.2 and 3.8 µg L-1 for Cd2+, respectively. Recoveries were between 75.5% and 117%, obtained by quantification via external calibration curves, thus eliminating the need for the laborious standard addition strategies.

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In this study, a novel apparatus for bar adsorptive microextraction (BAµE) using a voltage regulator was proposed as an alternative tool to improve the analysis throughput. In addition, recycled diatomaceous earth obtained as a brewery residue was employed as a biosorbent coating for the determination of methyl paraben, ethyl paraben, benzophenone and triclocarban in water samples by high-performance liquid chromatography-diode array detection (HPLC-DAD). The use of the extraction devices, comprised of floating adsorptive bars of 7.5mm length, in the extractions with magnetic stirrers linked to a voltage regulator enabled the analysis of multiple samples, simultaneously. The method optimization was carried out by univariate and multivariate analyses. The optimal conditions for the method were sample solution at pH 5, extraction time of 90min and liquid desorption in 100µL of acetonitrile:methanol (50:50, v/v) for 15min. The total sample preparation time was 17.5min per sample for a simultaneous batch of six extractions. The R2 values for the calibration curves obtained were higher than 0.9985. The limits of detection (LODs) varied from 0.19 to 2µgL-1 and the limits of quantification (LOQs) ranged from 0.63 to 6.9µgL-1. The method was applied to freshwater samples collected from Peri Lagoon (Florianópolis, SC, Brazil) and the relative recoveries ranged from 63% to 124% with relative standard deviations (RSDs) of < 20% (n = 2). The RSD values for the reproducibility of the performance of the magnetic stirrers and inter-device extraction efficiency were lower than 14% (n = 3) and 11% (n = 3), respectively.

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A combination of rotating disk sorptive extraction (RDSE) using Oasis® HLB as the sorbent phase and gas chromatography mass spectrometry (GC-MS) has been performed for the determination of four of the most widely used parabens: methylparaben, ethylparaben, propylparaben and n-butylparaben. The extraction and derivatization of the analytes in water samples were optimized by using factorial (screening) and Doehlert designs, thus reducing the number of analyses with the concomitant reduction of time, reagents, waste, samples and cost. Thus, a RDSE method using 20mL of sample was performed. The disk was rotated at 2900rpm for 70min at room temperature. After a desorption step and evaporation of solvent, a derivatization method using 5µL of N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) for 15min at room temperature was used previously to inject the final extract into GC-MS. The detection limits and precision (%RSD) were lower than 0.05µgL- 1 and 9.7% for the studied compounds, respectively. Recoveries were studied using effluent samples of a wastewater treatment plant (WWTP), with values higher than 80% being obtained. The applicability and reliability of this methodology were confirmed through the analysis of tap water and influents from Santiago, Chile, with concentration values ranging from 0.57 to 0.83µgL- 1 in influents. The main advantage of the present RDSE method is that it is significantly faster than its counterpart by SBSE and requires a considerable lower volume of derivatizing agent.

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