Bermudo E, Núñez O, Moyano E, Puignou L, Galceran M T
Department of Analytical Chemistry, University of Barcelona, Martí i Franquès, 1-11, E-08028 Barcelona, Spain.
J Chromatogr A. 2007 Aug 3;1159(1-2):225-32. doi: 10.1016/j.chroma.2007.03.008. Epub 2007 Mar 12.
This paper shows the applicability of capillary electrophoresis (CE) coupled to mass spectrometry (MS) for the analysis of acrylamide (AA) in foodstuffs. In order to obtain an ionisable compound amenable to be analysed by CE, acrylamide was derivatised with 2-mercaptobenzoic acid. Spectra in positive and negative modes were studied in order to select the best ionisation mode and multistep tandem mass spectrometry was used to obtain structural information. Maximum signal was observed when negative mode was used and MS/MS and MS3 were selected for quantitation and confirmation, respectively. For the separation, a fused-silica capillary of 80 cm and 50 microm I.D. and 35 mM ammonium formate/ammonia solution at pH 10 as running electrolyte were used. The applicability of field amplified sample injection (FASI) in reversed polarity was evaluated in order to decrease detection limits. The developed FASI-CE-MS/MS method provided a detection limit of 8 ng g(-1) and good linearity (r=0.999) and precision (day-to-day lower than 15%). The method has been applied to the analysis of different representative food products and the results were compared with those obtained by LC-MS/MS.
本文展示了毛细管电泳(CE)与质谱(MS)联用技术在食品中丙烯酰胺(AA)分析方面的适用性。为了获得适合CE分析的可电离化合物,丙烯酰胺用2-巯基苯甲酸进行衍生化。研究了正、负离子模式下的光谱,以选择最佳电离模式,并采用多步串联质谱法获取结构信息。使用负离子模式时观察到最大信号,分别选择MS/MS和MS3进行定量和确证。分离采用内径50μm、长80cm的熔融石英毛细管,以pH 10的35mM甲酸铵/氨溶液作为运行电解质。评估了反相极性下场放大进样(FASI)的适用性,以降低检测限。所建立的FASI-CE-MS/MS方法的检测限为8 ng g(-1),具有良好的线性(r = 0.999)和精密度(日间精密度低于15%)。该方法已应用于不同代表性食品的分析,并将结果与LC-MS/MS法获得的结果进行了比较。