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Technical University of Crete
Technical University of Crete
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| URI: | http://purl.tuc.gr/dl/dias/94F2519C-3630-4CAB-99B9-7CD9F163DF10 | ||
| Year | 2011 | ||
| Type of Item | Peer-Reviewed Journal Publication | ||
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| Bibliographic Citation | A. Papadopoulou, I. P Román, A. Canals, K. Tyrovola, E. Psillakis , 'Fast screening of perfluorooctane sulfonate in water using vortex-assisted liquid–liquid microextraction coupled to liquid chromatography–mass spectrometry " ,Anal. Chim. Acta,VOL. 691,no.1 , PP. 56–61,2011.doi :10.1016/j.aca.2011.02.043 https://doi.org/10.1016/j.aca.2011.02.043 | ||
| Appears in Collections |
Fast screening of trace amounts of the perfluorooctane sulfonate anion (PFOS) in water samples wasperformed following a simple, fast and efficient sample preparation procedure based on vortex-assistedliquid–liquid microextraction (VALLME) prior to liquid chromatography–mass spectrometry. VALLMEinitially uses vortex agitation, a mild emulsification procedure to disperse microvolumes of octanol, alow density extractant solvent, in the aqueous sample. Microextraction under equilibrium conditions isthus achieved within few minutes. Subsequently, centrifugation separates the two phases and restoresthe initial microdrop shape of the octanol acceptor phase, which can be collected and used for liquidchromatography–single quadrupole mass spectrometry analysis. Several experimental parameters werecontrolled and the optimum conditions found were: 50L of octanol as the extractant phase; 20mLaqueous donor samples (pH = 2); a 2 min vortex extraction time with the vortex agitator set at a 2500rpmrotational speed; no ionic strength adjustment. Centrifugation for 2 min at 3500rpm yielded separationof the two phases throughout this study. Enhanced extraction efficiencies were observed at low pHwhich was likely due to enhanced electrostatic interaction between the negatively PFOS molecules andthe positively charged octanol/water interface. The effect of pH was reduced in the presence of sodiumchloride, likely due to electrical double layer compression. The linear response range for PFOS was from5 to 500 ng L−1 (coefficient of determination, r2, 0.997) and the relative standard deviation for aqueoussolutions containing 10 and 500 ng L−1 PFOS were 7.4% and 6.5%, respectively. The limit of detection was1.6 ng L−1 with an enrichment factor of approximately 250. Analysis of spiked tap, river and well watersamples revealed that matrix did not affect extraction
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