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Title: Optimisation of an in-tube solid phase microextraction method coupled with HPLC for determination of some oestrogens in environmental liquid samples using different capillary columns
Authors: Aufartová, J.
Torres-Padron, M. E. 
Sosa-Ferrera, Z. 
Solich, P.
Santana-Rodríguez, J. J. 
UNESCO Clasification: 2301 química analítica
2391 Química ambiental
Keywords: Oestrogens
Eendocrine disruptor chemicals (EDCs)
In-tube SPME,
Sea water
Effluent of wastewater treatment plant, et al
Issue Date: 2012
Publisher: 0306-7319
Project: Desarrollo de Nuevas Estrategias de Extracción en El Análisis de Residuos Farmacéuticos.Implementación en Muestras Reales de Interés Medioambiental. 
Journal: International Journal of Environmental Analytical Chemistry 
Conference: 36th International Symposium on Environmental Analytical Chemistry 
Abstract: A simple on-line method for simultaneous determination of some oestrogens including oestriol (E3), norethisterone (NORE), ethynylestradiol (EE2), D-norgestrel (NORG) and bisphenol A (BPA), in environmental liquid samples was developed by coupling in-tube solid phase microextraction (in-tube SPME) to high-performance liquid chromatography with diode array (DAD) and fluorescence (FLD) detectors. Two capillary chromatographic columns (Supel-Q™ and Carboxen™ 1006 porous layer open tubular) were selected to develop this method. To achieve optimum extraction performance, several parameters were investigated including number of draw/eject cycles and the sample volume for each of the columns. Reproducibility was satisfactory for inter- and intra-day precision, yielding % RSDs of less than 10% and 7.6%, respectively. Limits of detection (LODs) and quantification (LOQs) for the proposed method using a DAD detector were achieved in the ranges of 0.04–0.63 ng mL−1 and 0.12–1.9 ng mL−1, depending of the capillary column used. Fluorescence detection improved these parameters for E3, BPA and EE2, obtaining LODs of 0.005–0.03 ng mL−1 and LOQs of 0.015–0.08 ng mL−1 using Supel-Q and LODs of 0.01–0.015 ng mL−1 and LOQs of 0.025–0.04 ng mL−1 using Carboxen. The proposed method was successfully applied to spiked environmental waters obtaining recoveries greater than 80%.
ISSN: 0306-7319
DOI: 10.1080/03067319.2011.585714
Source: International Journal Of Environmental Analytical Chemistry [ISSN 0306-7319], v. 92 (4), p. 382-396
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