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Expanded polystyrene (EPS) and polyurethane foams (PUFs) are widely produced and used due to their properties and, recently, it has been described that polystyrene present π–π interactions. Therefore, this work proposes to use recycled EPS to modify the surface of PUFs for the retention of 12 polycyclic aromatic hydrocarbons (PAHs) in air samples. PUF cylinders were modified with recycled polystyrene and characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, and affinity experiments. The proposed material is suitable for the retention-elution of PAHs from air samples, and can be incorporated to liquid chromatography generating a quantitative methodology. This methodology is efficient, fast and use lower volumes of organic solvents compared with other methodologies. Eighteen urban air samples were collected and analyzed weekly, using principal component analysis (PCA), and a relation between meteorological parameters and concentration of PAHs was observed. [ABSTRACT FROM AUTHOR]

Microcapsules of cellulose acetate with Cyanex 923 were prepared and used in this study for phenol removal from water and synthetic textile wastewater. The influence of several factors on the microcapsules extraction efficiency was studied, as well as characterization and phenol adsorption isotherm. Microcapsules characterization demonstrated the extractant reagent encapsulation, while in a batch mode procedure, good adsorption of phenol (ca. 5.5 × 10−3 mol Kg−1) has been reached. A slight decrease in phenol extraction percentage was obtained when synthetic textile wastewater was used (ca. 4.955 × 10−3 mol Kg−1), although a decrease in color was observed due to dye microcapsule extraction. Results indicate that this method is a promising alternative to conventional phenol removal technologies for aqueous samples of low phenol concentrations or in textile effluents. [ABSTRACT FROM AUTHOR]

To achieve analytical success, it is necessary to develop thorough clean-up procedures to extract analytes from the matrix. Dispersive solid phase extraction (DSPE) has been used as a pretreatment technique for the analysis of several compounds. This technique is based on the dispersion of a solid sorbent in liquid samples in the extraction isolation and clean-up of different analytes from complex matrices. DSPE has found a wide range of applications in several fields, and it is considered to be a selective, robust, and versatile technique. The applications of dispersive techniques in the analysis of veterinary drugs in different matrices involve magnetic sorbents, molecularly imprinted polymers, carbon-based nanomaterials, and the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. Techniques based on DSPE permit minimization of additional steps such as precipitation, centrifugation, and filtration, which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique and how it has been applied to food analysis. [ABSTRACT FROM AUTHOR]

Magnetic solid phase extraction has been used as pretreatment technique for the analysis of several compounds because of its advantages when it is compared with classic methods. This methodology is based on the use of magnetic solids as adsorbents for preconcentration of different analytes from complex matrices. Magnetic solid phase extraction minimizes the use of additional steps such as precipitation, centrifugation, and filtration which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique which were applied in food analysis. [ABSTRACT FROM AUTHOR]

Highlights: [•] A magnetic solid phase extraction method based on Fe3O4–SiO2–phenyl was developed. [•] This technique is based on the dispersion of a magnetic adsorbent in liquid samples. [•] Method developed was employed for the extraction of nine sulphonamides from milk. [•] The novel method was validated according European Decision 2002/657/EC. [•] Method demonstrated to be an efficient strategy for sulphonamides determination. [Copyright &y& Elsevier]

Abstract: A magnetic solid phase extraction method coupled to capillary electrophoresis is proposed for the determination of tetracycline, oxytetracycline, chlortetracycline and doxycycline in milk samples. Five different magnetic phenyl silica adsorbents covered with magnetite were synthesized by varying the molar ratio of phenyltrimethylsilane and tetramethylorthosilicate; these adsorbents were evaluated in terms of their pH and degree of hydrophobicity for tetracycline retention. The optimal, selected combination of conditions was a pH of 10.0 and a magnetic sorbent ratio of 4:1; under these conditions, the retention capacity ranged from 99.7% to 101.2% for the four tetracyclines analyzed. The elution conditions and initial sample volume of the proposed extraction method were also optimized, and the best results were obtained with 1×10−3 M acetic acid in methanol as eluent and a 200ml of sample volume. Under optimal conditions, average recoveries ranged from 94.2% to 99.8% and the limits of detection ranged from 2 to 9μgl−1 for the four tetracyclines. After the proposed method was optimized and validated, 25 milk samples of different brands were analyzed, oxytetracycline residues were detected in five samples, in concentrations ranging from 98 to 213μgl−1. Subsequent analysis of positive samples by SPE–CE and magnetic solid phase extraction–HPLC revealed than no significant differences were found from results obtained by the proposed methodology. Thus, the developed magnetic extraction is a robust pre-concentration technique that can be coupled to other analytical methods for the quantitative determination of tetracyclines. [Copyright &y& Elsevier]

• A method for the determination of malachite green and its leuco form was proposed. • The methodology consists on the use of modified henequen fibers as adsorbent in d-SPE. • The work proposes the use of copper phthalocyanine to modify the henequen fibers. • The methodology allowed the determination of both analytes using d-SPE-CE-DAD. • The methodology was applied in the analysis of fish samples with satisfactory results. A novel and simple procedure for the determination of malachite green (MG) and leuco-malachite green (LMG) in fish muscle was designed and validated. The method involved the use of henequen fibers modified with copper phthalocyanine as an efficient adsorbent in a dispersive-solid phase extraction technique. Following the extraction and pre-concentration process, CE-DAD was employed to quantify MG and LMG. The structural similarity of MG and LMG and the presence of the cationic forms under acidic conditions are the main drawbacks to determine these analytes in capillary electrophoresis. The proposed methodology allowed for the effective extraction and separation of both analytes using d-SPE-CE-DAD. The experimental parameters of the d-SPE technique were evaluated in order to get the highest pre-concentration efficiency. Under optimum conditions, the methodology achieves a limit of detection of 12.5 μg kg−1 for malachite green and 5.0 μg kg−1 for leuco-malachite green. Repeatability and reproducibility (%RSD n = 3) were less than 5.0% RSD in all cases, indicating that the method shows good precision for the analysis of real samples. In order to evaluate the accuracy of the method, the recovery was evaluated in tilapia samples at three concentration levels, recoveries varied from 88.7% to 109.5% for MG and from 65.3% to 88.8% for LMG. The method was validated and successfully applied to determine MG and LMG in fish samples. [ABSTRACT FROM AUTHOR]

Cellulose acetate is derived from cellulose and has the characteristics of biodegradability and reusability. So, it has been used for the elimination of toxic compounds capable of producing different diseases, such as cadmium, that result from human and industrial activity. For this reason, capsules functionalized with Cyanex 923 were prepared and characterized by FTIR spectroscopy, Energy Dispersive X-ray Spectroscopy (EDX), and SEM. The functionalized capsules were used for removing and recovering Cd(II) by modifying variables such as HCl concentration in the extraction medium and carrier content in the capsules, among others. The extraction of cadmium from battery leachates and the three isotherm models, Langmuir, Freundlich, and Dubinin Radushkevich, were also tested to model the cadmium removal process. The results showed a favorable physical sorption with a good capacity for extraction and the possibility of reusing the capsules for up to seven cycles without a decrease in the percentage of cadmium recovery. [ABSTRACT FROM AUTHOR]

Review: 75 refs. [ABSTRACT FROM AUTHOR]

Since lead is a highly toxic metal, it is necessary to detect its presence in different samples; unfortunately, analysis can be complicated if the samples contain concentrations below the detection limit of conventional analytical techniques. Solid phase extraction is a technique that allows the carrying out of a pre-concentration process and thus makes it easy to quantify analytes. This work studied the efficiency of sorption and preconcentration of lead utilizing polysulfone (PSf) fibers grafted with acrylic acid (AA). The best conditions for Pb(II) extraction were: pH 5, 0.1 mol L−1 of ionic strength, and 40 mg of sorbent (70% of removal). The sorbed Pb(II) was pre-concentrated by using an HNO3 solution and quantified using flame atomic absorption spectrometry. The described procedure was used to obtain a correlation curve between initial concentrations and those obtained after the preconcentration process. This curve and the developed methodology were applied to the determination of Pb(II) concentration in a water sample contained in a handmade glazed clay vessel. With the implementation of the developed method, it was possible to pre-concentrate and determine a leached Pb(II) concentration of 258 µg L−1. [ABSTRACT FROM AUTHOR]

A simple, fast and efficient on-line pre-concentration method (large-volume sample stacking) by capillary electrophoresis was proposed for determination of azo dyes residues (allura red [AR], sunset yellow [SY] and tartrazine [TAR]) in water samples. Pre-concentration variables involved in the system were optimised using of a Box–Bhenken design. Under the optimal conditions: injection time 150.0 s, pre-concentration time 120.0 s and reverse potential −8.0 kV, the proposed methodology improved the analytical sensibility achieving limits of detection of 21.0–41.4 µg L−1 with enrichment factors of 82.1–210.8 fold. The large-volume sample stacking-capillary electrophoresis method was validated and applied to determine azo dyes residues in 20 water samples (bottled, spring and tap water). Two samples were positive for sunset yellow and tartrazine with a concentration of 25.3 and 30.2 µg L−1 and % RSD less than 10.0% in all cases. [ABSTRACT FROM AUTHOR]

Solid-phase extraction in combination with large-volume sample stacking-capillary electrophoresis (SPE-LVSS-CE) was applied to measure chlortetracycline, doxycycline, oxytetracycline, and tetracycline in milk samples. Under optimal conditions, the proposed method had a linear range of 29 to 200 µg·L−1, with limits of detection ranging from 18.6 to 23.8 µg·L−1 with inter- and intraday repeatabilities < 10% (as a relative standard deviation) in all cases. The enrichment factors obtained were from 50.33 to 70.85 for all the TCs compared with a conventional capillary zone electrophoresis (CZE). This method is adequate to analyze tetracyclines below the most restrictive established maximum residue limits. The proposed method was employed in the analysis of 15 milk samples from different brands. Two of the tested samples were positive for the presence of oxytetracycline with concentrations of 95 and 126 µg·L−1. SPE-LVSS-CE is a robust, easy, and efficient strategy for online preconcentration of tetracycline residues in complex matrices. [ABSTRACT FROM AUTHOR]

method is presented for magnetic solid phase extraction (MSPE) of tetracyclines in milk samples. The method involves the extraction and clean-up by silica based magnetic support dispersion on non-pretreated milk samples, followed by the magnetic isolation and desorption of the analytes by acidified methanol. The tetracyclines eluted from the magnetic support were determined simultaneously by flow injection analysis with spectrophotometric detection. Under optimal conditions, the linear range of the calibration curve ranges from 0.03 to 0.60 mg L, with a limit of detection of 10 μg L. Recoveries were determined for milk spiked at levels from 0.15 to 0.60 mg L. Average recoveries ranged from 91.0 to 97.0%, with a precision of <5.0% in all cases. The method was validated by comparing the results with those obtained by MSPE-HPLC and SPE-HPLC. No significant differences were observed ( p < 0.05) [ABSTRACT FROM AUTHOR]

A magnetic solid phase extraction technique followed by liquid chromatography with a fluorescence detector for naproxen analysis in human urine samples was developed. The method includes the extraction of naproxen with a magnetic solid synthetized with magnetite and poly 4-vinylpriridine, followed by the magnetic separation of the solid phase and desorption of the analyte with methanol. Under optimal conditions, the linear range of the calibration curve was 0.05–0.60 μg L−1, with a limit of detection of 0.02 μg L−1. In all cases values of repeatability were lower than 5.0% with recoveries of 99.4 ± 1.3%. Precision and accuracy values are adequate for naproxen (Npx) analysis in urine samples. [ABSTRACT FROM AUTHOR]

In this work, a procedure using solid phase microextraction in combination with capillary electrophoresis was developed for the determination of oxytetracycline in milk samples. The method involves the synthesis of poly(1-allyl-3-methyl imidazolium) chloride film on a stainless-steel bar via electropolymerization and its use as an adsorbent for oxytetracycline (OT) by an ionic exchange mechanism. The coated fiber is then immersed in milk samples for retention of oxytetracycline residues, followed by elution, drying, and reconstitution before analysis with capillary electrophoresis. The proposed method achieves a limit of detection of 70 µg L−1 with adequate precision and uncertainty, making this methodology appropriate for the determination of OT in milk samples. The method was applied to the pre-concentration and quantification of oxytetracycline in ten commercial milk samples. Two tested samples were positive for the presence of oxytetracycline but the concentration was below the maximum residue limit according to the international normative standard. The proposed methodology was evaluated according to the Eco-Scale approach, and the total score of 51 indicated that the methodology proposed is both green and acceptable despite the multi-stage character. SPME-CE methodology allows us to perform the sample pre-treatment and determination of OT in an effective and greener way, decreasing the number of steps during the analysis and the generation of waste. [ABSTRACT FROM AUTHOR]