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Fast determination of aqueous fullerene C60 aggregates by vortex-assisted liquid-liquid microextraction and liquid chromatography-mass spectrometry

Zouboulaki Rodopi, Psyllaki Eleftheria

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Summary

This work presents a new, fast and simple method for the determination of fullerene C60 aggregates (nC60) in environmental waters by vortex-assisted liquid-liquid microextraction (VALLME) and liquid chromatography-mass spectrometry. Vortex agitation accelerated mass transfer from the aqueous sample into the octanol phase and resulted in a short extraction time. Moreover, lowering the pH of the aqueous sample and adding small amounts of salt destabilized nC60 aggregates and facilitated mass transfer into the octanol phase. Several experimental parameters were controlled and the optimum conditions found were: 50 μL octanol as the extractant phase; 20 mL water sample (pH = 4; 1% w:v NaCl); 5 min vortex mixing at 2650 rpm followed by 2 min centrifugation at 3500 rpm. The linearity of the method was found to be good within the range 0.25-2.50 μg L-1 (coefficient of determination, r2, 0.9908) and the limit of detection for a signal-to-noise ratio of 3 was 0.08 μg L-1. The relative standard deviations for aqueous solutions containing 0.50 and 2.00 μg L-1 of nC60 were 7% and 3% respectively. The developed method was also applied to tap and effluent wastewater samples spiked with nC60 and the mean relative recoveries were 90 and 79% respectively. Overall, the proposed method is a low-cost and easy to use procedure that allows rapid low-level environmental determination of aqueous fullerene aggregates whilst using small sample volumes and microvolumes of organic solvent.

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