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微型基质固相分散结合液相色谱-串联质谱法用于定量分析儿童使用或食用的化妆品和食品中的合成染料。

Miniaturized matrix solid-phase dispersion followed by liquid chromatography-tandem mass spectrometry for the quantification of synthetic dyes in cosmetics and foodstuffs used or consumed by children.

作者信息

Guerra Eugenia, Llompart Maria, Garcia-Jares Carmen

机构信息

Laboratory of Research and Development of Analytical Solutions (LIDSA), Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, Universidade de Santiago de Compostela, E-15782, Santiago de Compostela, Spain.

Laboratory of Research and Development of Analytical Solutions (LIDSA), Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, Universidade de Santiago de Compostela, E-15782, Santiago de Compostela, Spain.

出版信息

J Chromatogr A. 2017 Dec 22;1529:29-38. doi: 10.1016/j.chroma.2017.10.063. Epub 2017 Oct 27.

DOI:10.1016/j.chroma.2017.10.063
PMID:29128093
Abstract

Miniaturized matrix solid-phase dispersion (MSPD) followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) has been proposed for the simultaneous analysis of different classes of synthetic dyes in confectionery and cosmetics intended for or mostly consumed by children. Selected compounds include most of the permitted dyes as food additives as well as some of the most frequently used to color cosmetic products in accordance with the respective European directives. MSPD procedure was optimized by means of experimental design, allowing an effective, rapid and simple extraction of dyes with low sample and reagents consumption (0.1g of sample and 2mL of elution solvent). LC-MS/MS was optimized for good resolution, selectivity and sensitivity using a low ionic strength mobile phase (3mM NHAc-methanol). Method performance was demonstrated in real samples showing good linearity (R≥0.9928) and intra- and inter-day precision (%RSD≤15%). Method LODs were ≤0.952μgg and ≤0.476μgg for confectionery and cosmetic samples, respectively. Recoveries of compounds from nine different matrices were quantitative. The validated method was successfully applied to 24 commercial samples (14 cosmetics and 10 foods) in which 9 of the selected dyes were found at concentrations up to 989μgg, exceeding in some cases the regulated maximum permitted limits. A non-permitted dye, Acid Orange 7, was found in one candy.

摘要

已提出采用微型基质固相分散(MSPD)结合液相色谱串联质谱(LC-MS/MS)法,同时分析儿童专用或主要供儿童食用的糖果和化妆品中不同种类的合成色素。所选化合物包括大多数作为食品添加剂允许使用的色素,以及一些根据欧洲相关指令常用于化妆品着色的色素。通过实验设计对MSPD程序进行了优化,可有效、快速且简单地提取色素,样品和试剂消耗量低(0.1g样品和2mL洗脱溶剂)。使用低离子强度流动相(3mM醋酸铵-甲醇)对LC-MS/MS进行了优化,以实现良好的分离度、选择性和灵敏度。在实际样品中验证了该方法的性能,结果表明线性良好(R≥0.9928),日内和日间精密度(%RSD≤15%)。糖果和化妆品样品的方法检出限分别≤0.952μg/g和≤0.476μg/g。从九种不同基质中回收化合物的回收率均为定量。该经过验证的方法成功应用于24个商业样品(14种化妆品和10种食品),其中在某些样品中发现9种所选色素的浓度高达989μg/g,在某些情况下超过了规定的最大允许限量。在一块糖果中发现了一种禁用色素酸性橙7。

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