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Analysis of (Functionalized) Fullerenes in Water Samples by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry

Analysis of (Functionalized) Fullerenes in Water Samples by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry

Annemieke Kolkman, Erik Emke, Patrick S Bäuerlein, Andrea Carboni, Diem Truc Tran, Thomas L ter Laak, Annemarie P van Wezel, Pim de Voogt

Anal Chem. 2013 Jun 18;85(12):5867-74.

PMID: 23705858

Abstract:

One of the main challenges in environmental risk assessment of fullerenes is to develop analytical methods that detect and quantify fullerenes at low concentrations. In this paper we report on the development and optimization of a highly specific, robust, and relatively simple method for the quantitative determination of C60, C70, and six functionalized fullerenes, namely, [6,6]-phenyl-C61-butyric acid methyl ester, [6,6]-phenyl-C61-butyric acid butyl ester, [6,6]-phenyl-C61-butyric acid octyl ester, [6,6]-bis(phenyl)-C61-butyric acid methyl ester, [6,6]-thienyl-C61-butyric acid methyl ester, and [6,6]-phenyl-C71-butyric acid methyl ester ([70PCBM], in different aqueous matrixes. For this method fullerenes were extracted from the aqueous phase using solid-phase extraction (SPE), with subsequent analysis on a liquid chromatography-Orbitrap mass spectrometry (LC-Orbitrap MS) system. SPE was optimized by varying different conditions to improve recovery of all fullerenes. Different SPE column materials (C18, C18e, C8, CN) were tested, and recoveries appeared to be the highest for the C18-material. Recoveries were improved by adding NaCl to the water during extraction. Very low limit of detection (LOD) values were obtained for all compounds with this method, ranging from 0.17 ng/L for [70]PCBM to 0.28 ng/L for C60, and subsequent limit of quantitation (LOQ) values of 0.57-0.91 ng/L. Recoveries for the fullerenes were on average 120% in ultrapure and drinking water. Recoveries appeared to be lower, but still acceptable (e.g., >78%), in surface water. The developed approach is promising and will be applied, for example, in (1) environmental monitoring, (2) a more in-depth study of environmental fate and transformation products, and (3) studying water treatment efficiency of C60, C70, and the various functionalized fullerenes.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP571177689	[6,6]-Phenyl-C61 butyric acid octyl ester		571177-68-9	Price
LS76132	[6,6]-Thienyl C61 butyric acid methyl ester			Price

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