Simultaneous determination of selected endocrine disrupters (pesticides, phenols and phthalates) in water by in-field solid-phase extraction (SPE) using the prototype PROFEXS followed by on-line SPE (PROSPEKT) and analysis by liquid chromatography-atmospheric pressure chemical ionisation-mass spectrometry

Abstract

In this study, a new procedure, based on on-line solid-phase extraction (SPE) and analysis by liquid-chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS), has been developed for the simultaneous, multianalyte determination of 21 selected pesticides, phenols and phthalates in water. SPE was carried out on polymeric PLRP-s cartridges by percolating 20 mL-samples. For sample preconcentration, the performance of a prototype programmable field extraction system (PROFEXS) was evaluated against the commercial laboratory bench Prospekt system used for method development. The Profexs is designed for the automated on-site sampling, SPE preconcentration, and storage of up to 16 samples in SPE cartridges. These cartridges are further eluted and on-line analyzed with the Prospekt coupled to the chromatographic system. In the optimized method, where completely on-line SPE-LC-MS analysis of the samples is carried out with the Prospekt in the laboratory, detection limits lower than 100 ng/L, and satisfactory precision (relative standard deviations <25%) and accuracies (recovery percentages >75%) were obtained for most investigated compounds from the analysis of spiked Milli-Q water. The extraction efficiency achieved with the Profexs was comparable to that of the Prospekt for most compounds and somewhat lower for the most apolar analytes, probably due to adsorption on the pump filters. The completely on-line optimized method was applied to the analysis of surface water, ground water and drinking water from a waterworks in Barcelona. Some pesticides and phenols were found in both surface water and groundwater at ng/L or microg/L levels, but not in the final drinking water. Di(2-ethylhexyl)phthalate (DEHP) was present in all samples investigated, including blanks. To the author's knowledge, this is the first work describing the application of a fully automated on-line SPE-LC-MS method for the simultaneous analysis of pesticides, phenols, and phthalates in water, and the second one that examines the possibilities of the prototype Profexs for automated on-site SPE preconcentration of organic pollutants from water samples.

Emerging contaminants in surface waters and their relevance for the production of drinking water in Europe

“…Petrovic et al 2003;Rodrigues et al 2007;Kuster et al 2009;Loos et al 2009;Palma et al 2009;Vryzas et al 2009). The occurrence of pesticides in drinking water was investigated for water prepared from the Llobregat River and reported to be undetectable (Lopez-Roldan et al 2004) or below 100 ng/l (Kuster et al 2008). …”

Validation of UV Spectrophotometric and HPLC Methods for Quantitative Determination of Chlorpyrifos

“…Reduction in acetylcholinesterase activity to 10 ±20 % of normal activity in man results usually in death [5]. Different chromatographic methods for the determination of chlorpyrifos in food and environmental samples [6][7]. For example, limits of detection (LOD) between 0.05 and 0.5 ng/ml were reached using thin layer chromatography (TLC) [8]; also high performance liquid chromatography (HPLC) with LOD [9].…”

Phthalates in food and medical devices

“…Therefore, the concentration in surface and ground water are usually less than 10 ppb and rarely exceed 10 ppm (Hites, 1973;Lopez Roldan et al, 2004;Mihovec Grdic et al, 2002).…”