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Title: | Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry |
Author: | Astefanei, Alina Núñez Burcio, Oscar Galcerán Huguet, M. Teresa |
Keywords: | Ful·lerens Espectrometria de masses Cromatografia de líquids d'alta resolució Mostreig mediambiental Fullerenes Mass spectrometry High performance liquid chromatography Environmental sampling |
Issue Date: | 2-Sep-2014 |
Publisher: | Elsevier B.V. |
Abstract: | In this work, a method is proposed for the simultaneous analysis of several pristine fullerenes (C60, C70, C76, C78, and C84) and three C60-fullerene derivatives (N-methyl fulleropyrrolidine, [6,6]-Phenyl C61 butyric acid methyl ester and [6,6]-Phenyl C61 butyric acid buthyl ester) in environmental samples. The method involves the use of ultrahigh performance liquid chromatography coupled to atmospheric pressure photoionization mass spectrometry (UHPLC-APPI-MS) and allowed the chromatographic separation in less than 4.5 minutes. The product ions from tandem mass spectrometry studies of fullerene derivatives, were characterized and the most abundant one (m/z 720), corresponding to [C60]-¿, was selected for quantitation. Selected reaction monitoring (SRM at 0.7 m/z FWHM) by acquiring two transitions using both isotopic cluster ions [M]-¿ and [M+1]-¿ as precursor ions was proposed for quantitation and confirmation purposes. For pristine fullerenes, highly-selective selected ion monitoring (H-SIM) acquisition mode by monitoring the isotopic cluster ions [M]-¿ and [M+1]-¿ was used. Pressurized solvent extraction conditions were optimized in order to improve recoveries of the studied fullerene compounds from sediment samples. Values up to 87-92% for C60-fullerene derivatives and lower but still acceptable, 70-80%, for pristine fullerenes were obtained. Method limits of quantitation (MLOQs) ranging from 1.5 pg L-1to 5.5 ng L-1 in water samples and from 0.1 ng Kg-1 to 523 ng Kg-1 in sediments were obtained with good precision (relative standard deviations always lower than 13%). The applicability of the developed method was evaluated by analyzing several environmental samples such as sediments and pond water and the detected levels for C60-fullerene derivatives were of 0.1-2.7 ng Kg-1and 1.5-8.5 pg L-1, respectively. C60 and C70 were the only pristine fullerenes detected in the analyzed samples (0.1-7.2 ng Kg-1 in sediments and 9-330 pg L-1 in water pond samples). |
Note: | Versió postprint del document publicat a: http://dx.doi.org/10.1016/j.chroma.2014.08.089 |
It is part of: | Journal of Chromatography A, 2014, vol. 1365, p. 61-71 |
URI: | http://hdl.handle.net/2445/99043 |
Related resource: | http://dx.doi.org/10.1016/j.chroma.2014.08.089 |
ISSN: | 0021-9673 |
Appears in Collections: | Articles publicats en revistes (Enginyeria Química i Química Analítica) |
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642832.pdf | 1.28 MB | Adobe PDF | View/Open |
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