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新型衍生化方法用于食品中丙烯酰胺的 GC-ECD 测定的验证。

Validation of a novel derivatization method for GC-ECD determination of acrylamide in food.

机构信息

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

出版信息

Anal Bioanal Chem. 2013 Jul;405(18):6137-41. doi: 10.1007/s00216-013-7001-3. Epub 2013 May 10.

DOI:10.1007/s00216-013-7001-3
PMID:23660693
Abstract

This paper proposes a new method for quantitative analysis of acrylamide in cereal-based foods and potato chips. The method uses reaction with trifluoroacetic anhydride, and analyses the resulting derivative by use of gas chromatography with electron-capture detection (GC-ECD). The effects of derivatization conditions, including temperature, reaction time, and catalyst, on the acylation reaction were evaluated. Chromatographic analysis was performed on an SE-54 capillary column. Under the optimum conditions, good retention and peak response were achieved for the acrylamide derivative. The analytical method was fully validated by assessment of LODs and LOQs (1 ng g(-1) and 25 ng g(-1), with relative standard deviations (RSD) 2.1 and 3.6, respectively), linearity (R = 0.9935 over the range 0.03-10 μg g(-1)), and extraction recovery (>96%, with RSD below 2.0, for acrylamide spiked at 1, 20, 50, and 100 ng g(-1); 99.8% for acrylamide content >1000 ng g(-1)). The method requires no clean-up of the acrylamide derivative before injection. The method has been successfully used to determine acrylamide levels in different commercial cereal-based foods, French fries, and potato chips.

摘要

本文提出了一种新的方法,用于定量分析谷物食品和薯片 中的丙烯酰胺。该方法使用三氟乙酸酐反应,并用电子捕获检测气相色谱法(GC-ECD)分析生成的衍生物。评估了衍生化条件(包括温度、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,丙烯酰胺衍生物的保留和峰响应良好。通过评估 LODs 和 LOQs(分别为 1 ng g(-1)和 25 ng g(-1),相对标准偏差(RSD)分别为 2.1 和 3.6)、线性(0.03-10 μg g(-1)范围内 R=0.9935)和提取回收率(丙烯酰胺在 1、20、50 和 100 ng g(-1)时添加时,回收率>96%,RSD<2.0;丙烯酰胺含量>1000 ng g(-1)时回收率为 99.8%)对分析方法进行了充分验证。在进样前,无需对丙烯酰胺衍生物进行净化。该方法已成功用于测定不同商业谷物食品、薯条和薯片的丙烯酰胺含量。

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引用本文的文献

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Foods. 2021 Aug 30;10(9):2038. doi: 10.3390/foods10092038.
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Effects of blanching treatments on acrylamide, asparagine, reducing sugars and colour in potato chips.热烫处理对薯片丙烯酰胺、天冬酰胺、还原糖及色泽的影响
J Food Sci Technol. 2018 Oct;55(10):4028-4041. doi: 10.1007/s13197-018-3329-1. Epub 2018 Jul 31.