Petrarca Mateus Henrique, Rosa Maria Aparecida, Queiroz Sonia Claudia Nascimento, Godoy Helena Teixeira
Department of Food Science, Faculty of Food Engineering, University of Campinas (UNICAMP), 13083-862 Campinas, SP, Brazil.
Laboratory of Residues and Contaminants, Brazilian Agricultural Research Corporation, EMBRAPA Environment, 13820-000 Jaguariúna, SP, Brazil.
J Chromatogr A. 2017 Nov 3;1522:62-69. doi: 10.1016/j.chroma.2017.09.052. Epub 2017 Sep 23.
A liquid chromatography triple quadrupole mass spectrometry method was developed and validated for the simultaneous determination of acrylamide and 4-hydroxy-2,5-dimethyl-3(2H)-furanone (HDMF) in baby food. The sample preparation involves acetonitrile-based extraction combined with dispersive primary secondary amine (PSA) cleanup and cation-exchange solid-phase extraction (SPE), which promotes efficient removal of matrix interferences. Analytical selectivity and sensitivity were achieved for the quantification of acrylamide and HDMF in complex matrices such as fruit, cereal and milk-based baby foods; furthermore, adequate linearity (range 10-300μgkg) in solvent and matrix-matched calibration curves, and appropriate recoveries (94-110%) and precision (RSD≤10%), under repeatability and within-laboratory reproducibility conditions, were also obtained. Expanded measurement uncertainty was estimated at the 20μgkg level (limit of quantification) on the basis of data obtained from in-house validation, with values of 25.5 and 16.5% for acrylamide and HDMF, respectively. The fitness for purpose of developed method was verified by analyzing 15 commercial baby foods available in the Brazilian market. Acrylamide was detected in one plum-based baby food (35μgkg) while HDMF in 67% of the samples analyzed (levels between 25 and 262μgkg).
建立并验证了一种液相色谱三重四极杆质谱法，用于同时测定婴儿食品中的丙烯酰胺和4-羟基-2,5-二甲基-3(2H)-呋喃酮（HDMF）。样品制备包括基于乙腈的萃取，结合分散型伯仲胺（PSA）净化和阳离子交换固相萃取（SPE），可有效去除基质干扰。该方法对水果、谷物和牛奶基婴儿食品等复杂基质中的丙烯酰胺和HDMF进行定量分析时，具有良好的选择性和灵敏度；此外，在溶剂和基质匹配校准曲线中具有足够的线性（范围10 - 300μg/kg），在重复性和实验室内部再现性条件下，也获得了适当的回收率（94 - 110%）和精密度（RSD≤10%）。根据内部验证获得的数据，在20μg/kg水平（定量限）估计了扩展测量不确定度，丙烯酰胺和HDMF的值分别为25.5%和16.5%。通过分析巴西市场上15种市售婴儿食品，验证了所开发方法的适用性。在一种李子基婴儿食品中检测到丙烯酰胺（35μg/kg），而在67%的分析样品中检测到HDMF（含量在25至262μg/kg之间）。
