Improving analysis of apolar organic compounds by the use of a capillary titania-based column: Application to the direct determination of faecal sterols cholesterol and coprostanol in wastewater samples |
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Authors: | Y Moliner-Martinez R Herráez-HernándezC Molins-Legua P Campins-Falcó |
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Institution: | Department of Analytical Chemistry, Faculty of Chemistry, University of Valencia, C/ Dr. Moliner 50, E46100 Burjassot, Valencia, Spain |
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Abstract: | This article reports a new procedure for the direct determination of faecal sterols coprostanol and cholesterol in wastewater samples as tracers of human sewage contamination. The method combines in-tube solid-phase microextraction (IT-SPME) for analyte enrichment and capillary liquid chromatography (LC) for separation with diode array detection for identification and quantification. A titania-based polymeric capillary column and a conventional octadecyl silica (ODS) capillary column were evaluated and compared for their ability to separate the analytes. The titania-based column allowed the separation of the analytes in much shorter chromatographic times and with better chromatographic profiles, which in turn resulted in better detectability. In addition, IT-SPME allowed the direct injection into the chromatographic system of sample volumes as large as 200 μL, thus making unnecessary off-line clean-up and concentration steps. In such a way, the tested compounds could be directly analysed in less than 10 min, the limits of detection (LODs) being 10 and 1.2 μg/L for coprostanol and cholesterol, respectively. The reliability of the proposed method was tested by processing several wastewater samples. |
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Keywords: | In-tube solid-phase microextraction (IT-SPME) Reversed-phase TiO2 capillary column (RP-TiO2 capillary column) Sterols Wastewater samples |
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