RESUMO
The main objective of this study was to determine the occurrence of polycyclic aromatic hydrocarbons (PAHs) in surface water samples collected from different points along the stream that flows through the Campus of the Federal University of Santa Maria, RS-Brazil. Before reaching the campus, the water in the stream is already contaminated by wastewater discharged from the surrounding, and once inside the Campus, additional wastewater from a Gas Station situated close to the University hospital. A bench scale photodegradation experiment was conducted of the occurring traces of anthracene, phenanthrene and naphthalene, with the aid of a stirred tank reactor and polymer-supported TiO2 as a catalyst. To prevent loss of the low soluble analytes, it was necessary to add 5% and 10% acetonitrile, as an organic modifier of the synthetic aqueous solutions and real samples, respectively. An experimental design was employed and the best conditions for the photocatalysis of the aqueous solutions and real samples were pH 9 and pH 7, and 35°C and 30°C, respectively. Under optimized conditions, the analytes were completely degraded after 60 min of irradiation. The subproducts of the photocatalysis were identified through gas chromatography/mass spectrometry, and fragmentation routes were proposed. The mean concentrations of PAHs in the polluted surface water and hospital wastewater were relatively high: 3.9 ± 1.7 and 21.5 ± 2.8 µg L-1, respectively. A preliminary risk assessment revealed that the presence of anthracene requires particular attention. The risk posed by the occurrence of PAHs in the surface water and hospital wastewater samples confirms the need for an efficient treatment system.
Assuntos
Hospitais , Hidrocarbonetos Policíclicos Aromáticos/isolamento & purificação , Rios/química , Águas Residuárias/química , Poluentes Químicos da Água/isolamento & purificação , Brasil , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Fenantrenos/isolamento & purificação , Hidrocarbonetos Policíclicos Aromáticos/análise , Águas Residuárias/análise , Poluentes Químicos da Água/análise , Poluição da Água/análiseRESUMO
Statins are classified as being amongst the most prescribed agents for treating hypercholesterolaemia and preventing vascular diseases. In this study, a rapid and effective liquid chromatography method, assisted by diode array detection, was designed and validated for the simultaneous quantification of atorvastatin (ATO) and simvastatin (SIM) in hospital effluent samples. The solid phase extraction (SPE) of the analytes was optimized regarding sorbent material and pH, and the dispersive liquid-liquid microextraction (DLLME), in terms of pH, ionic strength, type and volume of extractor/dispersor solvents. The performance of both extraction procedures was evaluated in terms of linearity, quantification limits, accuracy (recovery %), precision and matrix effects for each analyte. The methods proved to be linear in the concentration range considered; the quantification limits were 0.45 µg L-1 for ATO and 0.75 µg L-1 for SIM; the matrix effect was almost absent in both methods and the average recoveries remained between 81.5-90.0%; and the RSD values were <20%. The validated methods were applied to the quantification of the statins in real samples of hospital effluent; the concentrations ranged from 18.8 µg L-1 to 35.3 µg L-1 for ATO, and from 30.3 µg L-1 to 38.5 µg L-1 for SIM. Since the calculated risk quotient was ≤192, the occurrence of ATO and SIM in hospital effluent poses a potential serious risk to human health and the aquatic ecosystem.
Assuntos
Inibidores de Hidroximetilglutaril-CoA Redutases/análise , Poluentes Químicos da Água/análise , Brasil , Cromatografia Líquida de Alta Pressão/métodos , Hospitais Universitários , Microextração em Fase Líquida/métodos , Extração em Fase Sólida/métodosRESUMO
A fast method for the determination of cocaine and its metabolites in hospital effluent samples was worked out by using liquid chromatography with the aid of fluorescence and diode array detection. Solid phase extraction and dispersive liquid -liquid microextraction were employed during the sample preparation stage. The experiment was conducted by using Chromabond® C18 ec 6 ml/500 mg cartridges, with recoveries higher than 96.6%, 88.3%, 78.7%, and LOQm 0.15; 0.18 and 0.30 µg L-1 for cocaine, benzoylecgonine and anhydroecgonine respectively. In the case of DLLME, different chemical conditions and solvent combinations were tested to find the best settings for the microextraction: pH 9; addition of 0.3 mol L-1 NaCl; 150 µL extractor (chloroform) and 350 µL disperser (methanol). The recoveries for cocaine were as high as 98.3% with LOQm 0.3 µg L-1. After validation, these methods were applied to quantification of the analytes. While the concentration of the anhydroecgonine, (the main pyrolytic metabolite of cocaine), remained below the limit of detection, the range of concentrations of cocaine and benzoylecgonine determined were 0.4-4.9 µg L-1 and 0.9-8.6 µg L-1, respectively. The occurrence has a relatively median/high environmental impact. These concentration values suggest that a role is played by other sources of cocaine, probably related to transport, or handling and the consumption of the drug. The outcome is that cocaine can be quantified by using DLLME as well as SPE, however, DLLME offered clear benefits like simplicity, affordability, and speed, as well as only requiring a small volume of solvents and samples.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Cocaína/análise , Hospitais Universitários , Drogas Ilícitas/análise , Microextração em Fase Líquida/métodos , Poluentes Químicos da Água/análise , Brasil , Calibragem , Cocaína/análogos & derivados , Cocaína/metabolismo , Drogas Ilícitas/metabolismo , Limite de Detecção , Metanol/química , Reprodutibilidade dos Testes , Risco , Extração em Fase Sólida/métodos , Solventes/química , Águas Residuárias/química , Poluentes Químicos da Água/metabolismoRESUMO
In this study, the preparation and application of extraction bars of PDMS were investigated to preconcentrate and determine benzene, toluene, ethylbenzene, and xylene in water and wastewater by means of HPLC with fluorescence detection. Aliquot samples from hospital wastewater were used as the model effluent. The independent variables for the sorptive extraction were as follows: ionic strength (added amounts of NaCl); pH; temperature and time of absorption; temperature and time of desorption. Under optimized conditions, by using a factorial design, the suspended extraction bars could allow the determination of benzene, toluene, ethylbenzene, and xylene (1.20 ± 0.05 µg/L; 10.40 ± 0.02 µg/L; 1.80 ± 0.04 µg/L; 15.9 ± 0.04 µg/L, respectively) in hospital effluent (fortified samples), by recoveries of 71.9 ± 4.9 to 74.8 ± 5.6%. This procedure represents an innovation that eliminates the time-consuming stage of vacuum microfiltration, and allows the determination of volatile organic compounds by HPLC. As far as we know, this procedure is original and represents an important contribution to the field.