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采用高效液相色谱-荧光检测法,用羟胺试剂对饮料中的低分子量醛进行高灵敏度分析。

Highly sensitive analysis of low-molecular-mass aldehydes in beverages using a hydroxylamine reagent by high-performance liquid chromatography with fluorescence detection.

机构信息

Department of Chemistry, School of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, Wuhan, 430070, China.

出版信息

Anal Bioanal Chem. 2022 Jul;414(17):5009-5022. doi: 10.1007/s00216-022-04132-1. Epub 2022 May 31.

Abstract

In this study, a fluorescent reagent, 4-((aminooxy)methyl)-7-hydroxycoumarin (AOHC), was for the first time applied to label the low-molecular-mass aldehydes (LMMAs) through reductive oxyamination reaction to afford single N,O-substituted oxyamine derivatives at room temperatures with derivatization efficiencies as high as 96.8%. In the following high-performance liquid chromatography with fluorescence detection analysis, 12 LMMAs, including furfurals, aromatic aldehydes, and aliphatic aldehydes, were baseline-separated on an ODS column and detected with low limits of detection (LODs) (0.2-50 nM), and good precisions (intraday relative standard deviations [RSDs] were 2.40-4.68%, and interday RSDs were 4.65-8.91%). This approach was then adopted to analyze six alcoholic beverages and five dairy products, and nine LMMAs with concentrations in the 0.28-798.16 μM range were successfully detected with excellent accuracies (recoveries were 92.2-106.2%). Finally, the results were statistically analyzed and discussed. The proposed method has several advantages, including high sensitivity, room-temperature labeling, and the avoidance of further extraction and/or enrichment procedures, demonstrating its great utility for monitoring LMMAs in various complex matrices.

摘要

在这项研究中,首次应用荧光试剂 4-((氨氧基)甲基)-7-羟基香豆素 (AOHC) 通过还原氨氧化反应标记低分子量醛 (LMMAs),在室温下以高达 96.8%的衍生化效率获得单一的 N,O-取代的肟衍生物。在随后的荧光检测高效液相色谱分析中,12 种 LMMAs(包括糠醛、芳香醛和脂肪醛)在 ODS 柱上基线分离,检测限低(0.2-50 nM),精密度良好(日内相对标准偏差 [RSD] 为 2.40-4.68%,日间 RSD 为 4.65-8.91%)。该方法随后用于分析六种酒精饮料和五种乳制品,成功检测到浓度范围在 0.28-798.16 μM 的九种 LMMAs,具有优异的准确性(回收率为 92.2-106.2%)。最后,对结果进行了统计分析和讨论。该方法具有灵敏度高、室温标记、避免进一步提取和/或富集步骤等优点,在各种复杂基质中监测 LMMAs 具有很大的应用价值。

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