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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Capillary liquid chromatography with diode array and mass spectrometry detection for heterocyclic aromatic amine determination in ready-to-eat food treated with electron-beam irradiation
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Capillary liquid chromatography with diode array and mass spectrometry detection for heterocyclic aromatic amine determination in ready-to-eat food treated with electron-beam irradiation

机译：二极管阵列毛细管色谱-质谱联用法检测电子束辐照即食食品中的杂环芳香胺

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摘要

In the present paper, we have developed a capillary liquid chromatography with MS detection for the determination at ngg~(-1) levels of four heterocyclic aromatic amines (MeIQx, norharman, harman and harmine), a group of mutagenic and carcinogenic compounds that can potentially be produced in protein-rich food during processing operations. They have been determined in commercial ready-to-eat (RTE) smoked salmon and soft cheese treated with E-beam irradiation. On the basis of experimental design studies and operating conditions of MS detector, best chromatographic conditions were obtained using a Luna~? C_(18) capillary column (150mm×0.3mm I.D.) with a mixture of acetonitrile-ammonium formate 5mM pH 3.6 buffer (13:87, v/v) as mobile phase. To improve sensitivity, large injection volumes (20μL) and injection solutions of low elution strength were employed. Sample preparation procedure included a previous treatment with 1M NaOH, followed by two solid-phase extraction steps; firstly on diatomaceous earth and then on mixed-mode cartridges. Heterocyclic amines were detected neither in irradiated and in non-irradiated samples, indicating that they were not formed by the radiation effect even at doses higher than those indicated in the Food Safety Objective established by regulatory agencies. RTE food samples were spiked at concentration levels in the range 10-30ngg~(-1). Recoveries higher than 85% (n=3 for each spiked level) were obtained, showing the effectiveness of the proposed methodology.
机译：在本文中，我们开发了一种毛细管液相色谱-质谱检测器，用于在ngg〜（-1）水平上测定四种杂环芳族胺（MeIQx，norharman，harman和harmine），这组诱变和致癌化合物可以可能在加工过程中以富含蛋白质的食物制成。它们已经在经电子束辐射处理的商用即食（RTE）烟熏三文鱼和软奶酪中确定。在实验设计研究和MS检测器的操作条件的基础上，使用LunaTM获得了最佳色谱条件。 C_（18）毛细管柱（150mm×0.3mm I.D.），以乙腈-甲酸铵5mM pH 3.6缓冲液（13:87，v / v）的混合物作为流动相。为了提高灵敏度，采用了大体积进样量（20μL）和低洗脱强度的进样溶液。样品制备程序包括预先用1M NaOH处理，然后进行两个固相萃取步骤;首先在硅藻土上，然后在混合模式滤筒上。在辐照和未辐照的样品中均未检测到杂环胺，这表明即使辐射剂量高于监管机构制定的《食品安全目标》中规定的剂量，它们也不是由辐射作用形成的。 RTE食品样品的加标浓度范围为10-30ngg〜（-1）。回收率高于85％（每个加标水平n = 3），表明了所提出方法的有效性。

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