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氮氧化物的形成:一种新的醛类衍生化策略及其在高效液相色谱荧光检测法测定食品中糠醛类物质中的应用。

Nitrone formation: A new strategy for the derivatization of aldehydes and its application on the determination of furfurals in foods 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, 430070 Wuhan, China.

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

出版信息

Talanta. 2018 Feb 1;178:834-841. doi: 10.1016/j.talanta.2017.10.027. Epub 2017 Oct 17.

Abstract

A nitrone formation method using a novel fluorescent reagent 4-hydroxylaminopropyl-7-methoxylcoumarin (HAMC) has been developed and applied for the determination of furfurals in foods using high performance liquid chromatography with fluorescence detection (HPLC-FLD). Furfurals samples were derivatized by HAMC in aqueous condition at room temperature in less than 30min and were subjected to direct HPLC-FLD analysis without extra purification or extraction. Compared with other conventional methods, nitrone formation method produced single chromatographic peak for each analyte, leading to simpler chromatograms and enhancing the overall sensitivity. Low detection limits at sub-nM level (0.08-0.1nM) and high repeatabilities (intra-day RSD ≤ 4.2% and inter-day RSD ≤ 6.7%) were achieved. The linear range of the calibration curve was 0.2-4000nM with good correlation coefficients (R ≥ 0.9989). This method was successfully applied for furfurals determination in food samples, including honey and coffee. The accuracy was satisfactory with recoveries ranging from 89.7% to 106.7% Above all, this pre-column derivatization method is simple, reliable and highly sensitive, providing a promising way for future studies of aldehydes from various sources.

摘要

开发并应用了一种新型荧光试剂 4-羟氨丙基-7-甲氧基香豆素(HAMC)的亚硝酮形成方法,用于使用带有荧光检测的高效液相色谱法(HPLC-FLD)测定食品中的糠醛。在室温下,HAMC 在水相中不到 30 分钟即可将糠醛样品衍生化,无需额外的纯化或提取,即可直接进行 HPLC-FLD 分析。与其他常规方法相比,亚硝酮形成方法为每个分析物产生单一色谱峰,导致色谱图更简单,整体灵敏度更高。在亚纳摩尔水平(0.08-0.1nM)下达到了低检测限和高重复性(日内 RSD≤4.2%,日间 RSD≤6.7%)。校准曲线的线性范围为 0.2-4000nM,相关系数良好(R≥0.9989)。该方法成功应用于食品样品(包括蜂蜜和咖啡)中糠醛的测定。回收率在 89.7%至 106.7%之间,准确度令人满意。总之,这种柱前衍生化方法简单、可靠、灵敏度高,为未来研究各种来源的醛类提供了一种有前途的方法。

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