University of Piemonte Orientale, DISAV Dipartimento di Scienze dell'Ambiente e della Vita, Viale T. Michel 11, 15121 Alessandria, Italy.
J Chromatogr A. 2011 Sep 16;1218(37):6308-18. doi: 10.1016/j.chroma.2011.06.085. Epub 2011 Jul 6.
An on-line solid phase extraction (SPE) ultra high performance liquid chromatography tandem mass spectrometry method has been developed for the simultaneous identification and determination of thirteen polycyclic aromatic hydrocarbons (PAHs) and twelve aldehydes (derivatized with 2,4-dinitrophenylhydrazine). The chromatographic conditions have been optimized to obtain the maximum of sensitivity and resolution taking into account the different retention interactions and the different ionization conditions of PAHs and derivatized aldehydes. LOD values ranging from 0.028 to 0.768 μg L(-1) for PAHs and from 0.002 to 0.125 μg L(-1) for aldehydes were obtained. The resolution permitted the separation of four couples of PAH isomers. Sample pre-treatment and SPE were optimized in order to apply the whole methodology to the analysis of different food matrices as salmon, frankfurter, steak, and pork chop, subjected to different cooking modes (smoked, grilled, cooked in oil or in butter). Particular attention was devoted to the evaluation of matrix effect that was significantly reduced through the on-line SPE treatment. For each food matrix the method detection limits, the method quantitation limits, and the recovery R were evaluated. R was shown not to depend on analyte concentration in the explored concentration range (LOQ - 50.000 μg L(-1)): the average R percent ranges from 70.6% to 120.0%.
已经开发出一种在线固相萃取 (SPE) 超高效液相色谱串联质谱法,用于同时鉴定和测定十三种多环芳烃 (PAHs) 和十二种醛(用 2,4-二硝基苯肼衍生化)。考虑到 PAHs 和衍生化醛的不同保留相互作用和不同的电离条件,优化了色谱条件以获得最大的灵敏度和分辨率。对于 PAHs,LOD 值范围为 0.028 至 0.768 μg L(-1),对于醛,LOD 值范围为 0.002 至 0.125 μg L(-1)。分辨率允许分离四对 PAH 异构体。优化了样品预处理和 SPE,以便将整个方法应用于不同食品基质(如三文鱼、法兰克福肠、牛排和猪排)的分析,这些食品经过不同的烹饪模式(熏制、烤制、油炸或油煎)。特别关注了基质效应的评估,通过在线 SPE 处理显著降低了基质效应。对于每种食品基质,评估了方法检测限、方法定量限和回收率 R。结果表明,R 不依赖于在探索浓度范围内(LOQ-50.000 μg L(-1)) 的分析物浓度:平均 R 百分比范围从 70.6%到 120.0%。