This work focuses on the validation and application of solid phase extraction followed by high-performance liquid chromatography (SPE-HPLC) analysis of important endocrine disruptors compounds (EDC) from different classes in highly complex wastewater matrix. The endocrine disruptors investigated included three different categories: pharmaceuticals (sulfamethoxazole (SMZ), trimethoprim (TMP) and diclofenac (DCF)), hormones (estrone (E1), 17α-ethinylestradiol (EE2) and 17β-estradiol (E2)) and plastic materials (bisphenol A (BPA)). The method involves pre-concentration by SPE using Strata-X extraction cartridges followed by HPLC coupled with diode array detector (DAD). As the assumption of homoscedasticity was met for analytical data, ordinary linear regression procedure was applied to the data. The method was considered validated for 7 EDC after consistent evaluation of the key analytical parameters. Recoveries were ranged from 52.3 to 179.6%. Limits of quantification were in the range 6.0-0.4 µg L−1. The described method was applied to evaluate the occurrence and removal efficiency of EDC in two biological sewage treatment plants (STPs). The influent mean concentrations of E1, E2 and EE2 hormones were 79.54; 175.09 and 102.19 µg L−1, respectively, while for SMZ, TMP, DCF and BPA were 215.17; 187.01; 218.97 and 87.12 µg L−1 for STP A, respectively. The efficiencies for the removal of EDCs ranged from 0 to 79.4%.
This paper investigates a strategy as a quality control parameter, using standard surrogate and determination of a relation factor for determination of parathion-methyl, chlorpyriphos and cypermethrin pesticides in environmental aqueous matrices with distinct characteristics (river water, estuarine, seawater and weir water), using the technique of solid phase microextraction gas chromatography with flame ionization detector (SPME-GC-FID). Pesticides were very susceptible to matrix effects promoted by environmental samples. The salinity and the organic matter seem to have been the main sources of interference in the method. For chlorpyriphos, in middle and high levels, the values of relation factor (Rf) for estuarines, seawater and weir matrices were statistically similar. For cypermethrin, the statistical equality occurred in estuarine matrices in medium and high levels of concentration. That indicates proportional behavior between the pesticide and the surrogate recovery, suggesting that a single value of Rf can be used as correction factor recovery for any of these matrices.
<p>Pesticides are used mostly in rural areas for agriculture, but urban pest control, public health campaigns, and household and veterinary products can also be important sources of these contaminants. This aim of this study was to estimate household pesticide contamination in sediments of two urban estuaries due to pest control: Cocó and Ceará rivers located in the metropolitan area of Fortaleza, Ceará, Brazil. Cypermethrin and malathion were found in both rivers. Cypermethrin levels had the same magnitudes as other studied urban areas and were highest in the estuary, while malathion was similar in both fluvial and estuarine zones.</p>
The first diagnosis of risk of environmental contamination was conducted for an area of intense agricultural activity in the semiarid cearense (Baixo Jaguaribe and Litoral de Aracati area). We verified the use of 201 rural products (pesticides) in the region, comprising 151 active ingredients. Regarding the active ingredients evaluated, 15.9% were associated with sediment and 29.8% were dissolved in surface water. The study showed that 13.2% to 36.4% of the active ingredients evaluated were classified as potential contaminants of groundwater resources. The study also revealed the most abundant pesticides and which environmental compartment must be evaluated.
The asphalt binder, derived from petroleum, commonly employed in road paving contains PAHs (Polycyclic Aromatic Hydrocarbons) and a variety of other aliphatic and aromatic compounds. PAHs are pollutants that can induce health problems. This work aims to extract and characterize the PAHs in samples of asphalt binder and its concentration. Matrix solid phase dispersion was used as a technique for extraction of the PAHs. Characterization was performed employing gas chromatography and scanning tunneling microscopy. Fifteen of the priority PAHs listed by USEPA (United States Environmental Protection Agency), as well as coronene, were found in the binder samples.
O ligante asfáltico de petróleo é comumente empregado na pavimentação de ruas e estradas de rodagem. Esse material contém hidrocarbonetos policíclicos aromáticos (HPAs) e diversos outros componentes alifáticos e aromáticos. Os HPAs são compostos poluentes que podem induzir problemas de saúde. Este trabalho tem como objetivo extrair e caracterizar os HPAs presentes no ligante asfáltico e suas concentrações. Dispersão de Matriz em Fase Sólida foi utilizada como técnica para a extração dos HPAs. Para análise e caracterização foram utilizadas as técnicas de Cromatografia Gasosa e Microscopia de Tunelamento. Quinze dos HPAs prioritários listados pela USEPA (United States Environmental Protection Agency) e também coroneno foram encontrados nas amostras analisadas.
Extraction and clean-up are essential points in polycyclic aromatic hydrocarbon (PAHs) analysis in a solid matrix. This work compares extraction techniques and clean-up procedures for PAH analysis. PAH levels, their toxicological significance and source were also evaluated in the waters of the Cocó and Ceará rivers. The efficiency of PAH recovery was higher for the soxhlet and ultrasonic techniques. PAH recovery varied from 69.3 to 99.3%. Total PAH concentration (ΣHPA) varied from 720.73 to 2234.76 µg kg-1 (Cocó river) and 96.4 to 1859.21 µg kg-1 (Ceará river). The main PAH sources are pyrolytic processes and the levels were classified as medium so that adverse effects are possible.
Green coconut shells were treated with acid, base and hydrogen peroxide solutions for 3, 6, 12 and 24 h for removing toxic metals from synthetic wastewater. The removal of ions by the adsorbent treated with 0.1 mol L-1 NaOH/ 3h was 99.5% for Pb2+ and 97.9% for Cu2+. The removal of Cd2+, Ni2+, Zn2+, using adsorbent treated with 1.0 mol L-1 NaOH/3 h, was 98.5, 90.3 and 95.4%, respectively. Particle size, adsorbent concentration and adsorption kinetics were also studied. An adsorbent size of 60-99 mesh and a concentration of 30-40 g/L for 5 min exposure were satisfactory for maximum uptake of Pb2+, Ni2+, Cd2+, Zn2+ and Cu2+ and can be considered as promising parameters for treatment the aqueous effluents contaminated with toxic metals.
Polycyclic aromatic hydrocarbons (PAHs) are a great environmental concern mainly because of their toxic, mutagenic and carcinogenic potential. This paper reports utilization of the solid-phase extraction (SPE) technique to determine PAHs in environmental aqueous matrices. The recovery from environmental aqueous matrices fortified with PAHs varied from 63.7 to 93.1% for atmospheric liquid precipitation, from 38.3 to 95.1% for superficial river water, and from 71.0 to 95.5% for marine water. No negative matrix effect was observed for the recovery of PAHs from atmospheric liquid precipitation and marine water, but was observed for superficial river water, particularly for PAHs possessing 5 and 6 aromatic rings.