Quantitative trace analysis of fullerenes in river sediment from Spain and soils from Saudi Arabia

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RESEARCH PAPER

Quantitative trace analysis of fullerenes in river sediment from Spain and soils from Saudi Arabia Josep Sanchís & Dalibor Božović & Naif A. Al-Harbi & Luis F. Silva & Marinella Farré & Damià Barceló

Received: 2 December 2012 / Revised: 12 March 2013 / Accepted: 15 March 2013 / Published online: 2 April 2013 # Springer-Verlag Berlin Heidelberg 2013

Abstract A quantitative method based on ultrasound-assisted toluene extraction followed by liquid chromatography– electrospray ionization–tandem mass spectrometry for the analysis of C60 and C70 fullerenes, N-methylfulleropyrrolidine, [6, 6]-phenyl C61 butyric acid methyl ester and [6, 6]-thienyl C61 butyric acid methyl ester has been developed. The method was validated using fortified blank river sediments according to the criteria of Commission Decision 2002/657/EC. The method limits of detection ranged from 14 to 290 pg/g, making it suitable for its application in environmental analysis. The method has been applied to investigate fullerene content in 58 soil samples collected from different urban and industrial areas in Saudi Arabia and in river sediment from six different sites in the Llobregat River Basin. In addition, in the case of the Llobregat River, superficial water samples from the same sites

Published in the special paper collection Liquid Chromatography— Tandem Mass Spectrometry with guest editors Damià Barceló and Mira Petrovic. Electronic supplementary material The online version of this article (doi:10.1007/s00216-013-6924-z) contains supplementary material, which is available to authorized users. J. Sanchís : D. Božović : M. Farré (*) : D. Barceló Institute of Environmental Assessment and Water Research (IDAEA-CSIC), C/Jordi Girona, 18-26, 08034 Barcelona, Catalonia, Spain e-mail: [email protected] N. A. Al-Harbi King Saud University, P.O. Box 2455, 11451 Riyadh, Saudi Arabia L. F. Silva Centro Universitario La Salle, Ensino, Av. Victor Barreto, 2288, Centro, 92000-010 Canoas, RS, Brazil D. Barceló Catalan Institute of Water Research (ICRA), C/Emili Grahit, 101, 17003 Girona, Catalonia, Spain

of the sediments were collected and analysed using a previous method. In soils from Saudi Arabia, C60-fullerene was the only compound that was detected and quantified in 19 % of samples. In the sediments of the Llobregat River, C60-fullerene was also the only one detected (33 % of the samples), while in river water, C70-fullerene was the most frequent compound, and it was quantified in 67 % of the samples. However, C60-fullerene was present in two of the six samples, but at higher concentrations than C70-fullerene, ranging from 0.9 to 7.8 ng/L. Keywords Fullerene . Soils . Sediments . Liquid chromatography–mass spectrometry

Introduction Fullerenes are carbon-based nanomaterials in hollow spherical shapes that have been gaining scientific attention as emerging contaminants during the recent years [1, 2]. The main sources of fullerenes in the environment are: natural events, such as volcanic activity [3]; anthropogenic incidental sources, like ind