Solid phase extraction using molecular imprinting polymers (MISPE) for the determination of estrogens in surface water by HPLC

Abstract

Estrogens are emerging pollutants and traditional sewage treatments unable to remove them. They are harmful to human health and to the environment. It is therefore important to evaluate the presence and concentration of estrogens in water bodies and environmental matrices. This work presents the development and application of a methodology for the determination of E1, E3, EE2 and E2 in surface waters using solid phase extraction with molecular imprinting polymers (MISPE) followed by identification and quantification by HPLC-DAD. Acetonitrile and water deionized acidified with phosphoric acid pH 3 (1:1, v/v), a flow rate of 1.0 ml min and the method was satisfactory for specificity and selectivity tests using caffeine, which is often found in water bodies receiving effluent, and DES, an estrogen used in the treatment of prostate cancer. Selected samples underwent cleanup and pre-concentration treatments using solid phase extraction with commercial phase (C18) and molecularly imprinted polymers (MISPE). The analysis of MISPE extracts indicate that it is possible to obtain results with greater sensitivity and precision for analyses of complex environmental matrices, demonstrating that the developed method can be applied in complex environmental matrices.Keywords: emerging pollutants, endocrine disruptors, environmental matrices.Extração em fase sólida utilizando polímeros de impressão molecular (MISPE) para a determinação de estrógenos em águas superficiais por HPLC RESUMOEstrogênios são poluentes emergentes e os tratamentos de esgoto tradicionais não são capazes de removê-los. São prejudiciais à saúde humana e ao ambiente. Portanto, torna-se 381 Solid phase extraction using molecular imprinting polymers (MISPE)… Rev. Ambient. Água vol. 12 n. 3 Taubaté -May / Jun. 2017 importante avaliar a presença e concentração dessas substâncias em corpos hídricos e matrizes ambientais. No presente trabalho, apresenta-se o desenvolvimento e aplicação de uma metodologia para a determinação de E1, E3, EE2, E2 em águas superficiais utilizando a extração em fase sólida com polímeros de impressão molecular (MISPE) seguida da identificação e quantificação via HPLC-DAD. A fase móvel empregada foi acetonitrila e água acidificada, com ácido fosfórico, pH 3, (1:1, v/v), vazão 1,0 mL min e o método mostrou-se satisfatório para testes de especificidade e seletividade usando cafeína encontrada em corpos hídricos que recebem efluentes, e DES, estrogênio utilizado em tratamento de câncer de próstata. Amostras selecionadas foram submetidas a clean-up e pré-concentração utilizando extração em fase sólida com fase comercial (C18) e polímeros de impressão molecular (MISPE). Os extratos MISPE analisados indicaram que é possível obter resultados com maior sensibilidade e precisão para análises de matrizes ambientais complexas; mostrando que o método desenvolvido pode ser aplicado em matrizes ambientais complexas.Palavras-chave: disruptores endócrinos, matrizes ambientais, poluentes emergentes.

Molecularly Imprinted Polymers for the Selective Extraction of Bisphenol A and Progesterone from Aqueous Media

“…MIPs have already proved their efficiency in selective preconcentration and measurements of endocrine disruptors in complex samples, such as ground water, milk, and serum [32,33,34,35]. In the detection of BPA, MIPs were used in several different formats, e.g., as a stationary phase in the capillary electrophoresis [31], superparamagnetic surface modified nanoparticles [36], or bulk materials combined with liquid chromatography-mass detection [37]. Despite many attempts of the synthesis and application of MIPs, they always suffered from low performance, complicated data analysis, and high batch variability.…”

Ultrasound-assisted dispersive liquid-liquid microextraction for determination of enrofloxacin in surface waters

“…In the field of environmental analysis, there are many protocols for enrichment and clean-up of water samples: liquid-liquid extraction [22], solid-phase extraction [23],…”