RESUMO
A molecularly imprinted polymer for the selective determination of Di(2-ethylhexyl) phthalate (DEHP) in water was synthesized and evaluated. This was accomplished by the use of sodium methacrylate as the monomer, toluene as a porogen, ethylene glycol dimethacrylate as a crosslinker, azobisisobutyronitrile as initiator and DEHP as a template molecule to generate the selectivity of the polymer for the compound, as well as synthesizing non-imprinted polymers. Three different polymerization approaches were used, emulsion, bulk and co-precipitation, the polymers obtained by emulsion presented a high retention rate reaching 99%. The method was able to pre-concentrate DEHP in water samples up to 250 times. To evaluate the applicability of the method, concentrations in fortified and bottled water were assessed using our polymer and determining DEHP concentrations by gas chromatography with mass spectrometry. Reported concentrations in bottled water were 12.1 µg/L, well above reference values established by the U.S. Environmental Protection Agency.
Assuntos
Dietilexilftalato/análise , Impressão Molecular/métodos , Polímeros , Poluentes Químicos da Água/análise , Água Potável/química , Cromatografia Gasosa-Espectrometria de Massas , Metacrilatos/química , Nitrilas/química , Polímeros/síntese química , Polímeros/química , Extração em Fase Sólida/métodos , Tolueno/químicaRESUMO
A molecularly imprinted polymer was developed and evaluated for selective determination of metronidazole (MNZ) in wastewater. This was achieved by using sodium methacrylate as monomer, toluene as porogen, ethylene glycol dimethacrylate as crosslinker, azobisisobutyronitrile as initiator and metronidazole as template molecule to generate the selectivity of the polymer for the compound, as well as non-imprinted polymers were synthesized. Two different polymerization approaches were used, bulk and emulsion and the polymers obtained by emulsion presented higher retention percentages the MIP 2-M presented the higher retention (83%). The performed method, was validated in fortified water, showing linearity from 10 up to 1000 ng/mL; limit of detection and quantification for compound were between 3 and 10 ng/mL, respectively. Finally, the method was applied in samples of a wastewater treatment plant in the city of San Luis Potosí, México, and the concentrations of MNZ in these samples were 84.1-114 ng/mL.
Assuntos
Metronidazol/análise , Impressão Molecular/métodos , Ácidos Polimetacrílicos/síntese química , Águas Residuárias/química , Poluentes Químicos da Água/análise , Adsorção , Limite de Detecção , Metacrilatos/química , México , Nitrilas/química , Ácidos Polimetacrílicos/química , Propriedades de Superfície , Tolueno/químicaRESUMO
In this work, a novel molecularly imprinted polymer (MIP) for use as a solid phase extraction sorbent was developed for the determination of coenzyme Q10 (CoQ10) in liver extract. CoQ10 is an essential cofactor in mitochondrial oxidative phosphorylation and a powerful antioxidant agent found in low concentrations in biological samples. This fact and its high hydrophobicity make the analysis of CoQ10 technically challenging. Accordingly, a MIP was synthesised using coenzyme Q0 as the template, methacrylic acid as the functional monomer, acetonitrile as the porogen, ethylene glycol dimethacrylate as the crosslinker and benzoyl peroxide as the initiator. Various parameters affecting the polymer preparation and extraction efficiency were evaluated. Morphological characterisation of the MIP and its proper comparison with C18 as a sorbent in solid phase extraction were performed. The optimal conditions for the molecularly imprinted solid phase extraction (MISPE) consisted of 400 µL of sample mixed with 30 mg of MIP and 600 µL of water to reach the optimum solution loading. The loading was followed by a washing step consisting of 1 mL of a 1-propanol solution (1-propanol:water, 30:70,v/v) and elution with 1 mL of 1-propanol. After clean-up, the CoQ10 in the samples was analysed by high performance liquid chromatography. The extraction recoveries were higher than 73.7% with good precision (3.6-8.3%). The limits of detection and quantification were 2.4 and 7.5 µg g(-1), respectively, and a linear range between 7.5 and 150 µg g(-1) of tissue was achieved. The new MISPE procedure provided a successful clean-up for the determination of CoQ10 in a complex matrix.