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Non-aqueous capillary electrophoresis separation of fullerenes and C60 fullerene derivatives

机译:富勒烯和C60富勒烯衍生物的非水相毛细管电泳分离

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摘要

As the interest in the use of fullerene compounds in biomedical and cosmetic applications increases, so too does the need to develop methods for their determination and quantitation in such complex matrices. In this work we studied the behavior of C60 and C70 fullerenes in non-aqueous capillary electrophoresis, as well as two C60 fullerene derivatives not previously reported by any electrophoretic method, N-methyl-fulleropyrrolidine (C60 pyrr) and (1,2-methanofullerene C60)-61-carboxylic acid (C60-COOH). . The separation was performed using fused-silica capillaries with an I.D. of 50 µm and tetraalkylammonium salts, namely tetra-n-decylammonium bromide (TDAB, 200 mM) and tetraethylammonium bromide (TEAB, 40 mM), in a solvent mixture containing 6% methanol and 10% acetic acid in acetonitrile:chlorobenzene (1:1 v/v) as the background electrolyte (BGE). Detection limits, based on a signal-to-noise ratio of 3:1, were calculated and values between 1 and 3.7 mg/L were obtained. Good run-to-run and day-to-day precisions on concentration were achieved with RDSs lower than 15%. For the first time, an electrophoretic technique (NACE) has been applied for the analysis of C60 fullerene in a commercial cosmetic cream. A standard addition method was used for quantitation and the result was compared with that obtained by analyzing the same cream by LC-MS.
机译:随着在生物医学和化妆品应用中使用富勒烯化合物的兴趣增加,对开发在此类复杂基质中测定和定量其方法的需求也随之增加。在这项工作中,我们研究了C60和C70富勒烯在非水毛细管电泳中的行为,以及以前没有任何电泳方法报道过的两种C60富勒烯衍生物,即N-甲基-全氟吡咯烷(C60 pyrr)和(1,2-甲基富勒烯C60)-61-羧酸(C60-COOH)。 。使用具有I.D.的熔融石英毛细管进行分离在含有6%甲醇和10%乙酸的乙腈:氯苯的混合溶剂中混合50μm和四烷基铵盐,即四正癸基溴化铵(TDAB,200 mM)和四乙基溴化铵(TEAB,40 mM)(1: 1 v / v)作为背景电解质(BGE)。基于3:1的信噪比,计算出检测限,得出的值介于1和3.7 mg / L之间。 RDS低于15%时,可以实现良好的逐次运行和日常浓度精度。电泳技术(NACE)首次用于商业美容霜中C60富勒烯的分析。使用标准添加方法进行定量,并将结果与​​通过LC-MS分析相同的乳霜得到的结果进行比较。

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