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通过气相色谱与电子俘获和离子阱质谱检测器联用,将常规谷物食品和薯片的丙烯酰胺快速简单地转化为 3-[双(三氟乙酰胺基)]-3-氧代丙基三氟乙酸酯进行测定。

Rapid and simple determination of acrylamide in conventional cereal-based foods and potato chips through conversion to 3-[bis(trifluoroethanoyl)amino]-3-oxopropyl trifluoroacetate by gas chromatography coupled with electron capture and ion trap mass spectrometry detectors.

机构信息

Department of Agriculture, Environment and Food, University of Molise, via De Sanctis, 86100 Campobasso, Italy.

出版信息

Food Chem. 2014 Mar 1;146:204-11. doi: 10.1016/j.foodchem.2013.09.050. Epub 2013 Sep 18.

DOI:10.1016/j.foodchem.2013.09.050
PMID:24176333
Abstract

A new, simple, rapid and fully validated method based on gas chromatography coupled with Electron capture and ion trap mass spectrometry detectors (GC-ECD and GC-IT/MS) is presented for quantitative analysis of acrylamide contaminant in conventional cereal-based foods and potato chips. Before analysis acrylamide was efficiently derivatized with trifluoroacetic anhydride, the effects of temperature, reaction time and catalyst on the acylation reaction were evaluated. Chromatographic analysis was performed on SE-54 capillary column; good retention and peak response of the acrylamide derivative achieved under the optimal conditions. The analytical method has been fully validated by assessment of the following parameters: LODs and LOQs (1 and 25ngg(-1) by GC-ECD and 2 and 36ngg(-1) by GC-IT/MS, with a Relative Standard Deviations <4 and <6, respectively), linearity (R(2) above 0.981 in the range 0.005-50μgg(-1)) and extraction recovery (ranging between 91% and 99%, RSD below 4.0, for acrylamide spiked at levels of 1, 20, 50 and 100ngg(-1)). Furthermore, the method proposed requires no clean-up step of the acrylamide derivative to be performed prior to injection. The developed method has been successfully applied to determine acrylamide in different commercial cereal-based foods (including French fries and potato chips).

摘要

一种新的、简单、快速且完全经过验证的方法,基于气相色谱法与电子捕获和离子阱质谱检测器(GC-ECD 和 GC-IT/MS)联用,用于定量分析传统谷物食品和薯片的丙烯酰胺污染物。在分析之前,丙烯酰胺通过三氟乙酸酐有效地衍生化,评估了温度、反应时间和催化剂对酰化反应的影响。在 SE-54 毛细管柱上进行色谱分析;在最佳条件下,丙烯酰胺衍生物实现了良好的保留和峰响应。通过评估以下参数对分析方法进行了充分验证:LODs 和 LOQs(GC-ECD 为 1 和 25ngg(-1),GC-IT/MS 为 2 和 36ngg(-1),相对标准偏差分别小于 4 和 6)、线性(在 0.005-50μg g(-1)范围内 R(2)大于 0.981)和提取回收率(丙烯酰胺在 1、20、50 和 100ng g(-1)水平下的加标回收率在 91%至 99%之间,RSD 低于 4.0)。此外,所提出的方法在注入之前不需要对丙烯酰胺衍生物进行净化步骤。该方法已成功应用于测定不同商业谷物食品(包括薯条和薯片)中的丙烯酰胺。

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