Institute of Environmental Assessment and Water Research (IDAEA-CSIC), C/Jordi Girona, 18-26, 08034, Barcelona, Catalonia, Spain.
Anal Bioanal Chem. 2013 Jul;405(18):5915-23. doi: 10.1007/s00216-013-6924-z. Epub 2013 Apr 2.
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 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.
建立了一种基于超声辅助甲苯提取，结合液相色谱-电喷雾串联质谱分析 C60 和 C70 富勒烯、N-甲基富勒吡咯烷、[6,6]-苯基 C61 丁酸甲酯和[6,6]-噻吩基 C61 丁酸甲酯的定量方法。该方法按照委员会 2002/657/EC 号决定的标准，使用加标空白河沉积物进行了验证。方法检出限范围为 14 至 290 pg/g，适用于环境分析。该方法已应用于调查沙特阿拉伯不同城市和工业区采集的 58 个土壤样品和六处不同地点的 Llobregat 河流域的河沉积物中的富勒烯含量。此外，在 Llobregat 河的情况下，还采集了来自沉积物相同地点的地表水样品，并使用先前的方法进行了分析。在沙特阿拉伯的土壤中，C60 富勒烯是唯一在 19%的样本中检测到并定量的化合物。在 Llobregat 河的沉积物中，也只检测到 C60 富勒烯（占样本的 33%），而在河水中，C70 富勒烯是最常见的化合物，在 67%的样本中进行了定量。然而，在六个样本中的两个样本中发现了 C60 富勒烯，但浓度高于 C70 富勒烯，范围从 0.9 到 7.8 ng/L。
