First determination of fullerenes in the Austrian market and environment: quantitative analysis and assessment

Abstract

This study forms the first report on analyzing fullerenes in the Austrian environment and cosmetic products available on the Austrian market. We developed, optimized, and validated a novel method for the analysis of C₆₀ and C₇₀ fullerenes and N-methylfulleropyrrolidine C₆₀ (NMFP) for measuring sensitivities in the low nanograms per liter range in order to prove their presence in the environment (12 wastewater- and 12 sewage sludge samples) and in 11 selected fullerene-containing cosmetic products from three different brands. The optimized method relies on a liquid-liquid extraction (LLE) or solid-liquid extraction (SLE) and, for the first time, introduced the Carrez-clarification, followed by liquid chromatography (LC) and coupled to a hybrid triple quadrupole mass spectrometry (MS) quantification. The total variability of the new established LC-MS/MS method based on all the tested matrices was below 10%. We found recoveries generally higher than 70% for both tap water and surface water. The limits of quantitation (LOQ) for the wastewater samples were measured to be from 0.8 to 1.6 ng/L, for the sewage sludge samples, from 1.4 to 2.6 ng/g DM (drymass), and for the cosmetic samples from 0.2 to 0.4 ng/g. None of the analyzed samples of wastewater or sewage sludge samples contained fullerenes. But in 70% of the tested cosmetics, fullerene concentrations between 10 and 340 ng/g were detected. These values were much lower than concentrations causing toxicity in water animals.