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基于偶合反应的 TLC 和 SERRS 联用鉴定 N-甲基苯胺。

Identification of N-methylaniline based on azo coupling reaction by combining TLC with SERRS.

机构信息

School of Pharmacy, Qiqihar Medical University , Qiqihar 161006,China.

School of Pharmacy, Qiqihar Medical University , Qiqihar 161006,China.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2021 May 5;252:119490. doi: 10.1016/j.saa.2021.119490. Epub 2021 Jan 21.

Abstract

The objective of this study was to establish a novel method for the determination of N-methylaniline (NMA) based on azo coupling reaction in infant pacifiers prepared with food contact silicone materials by combining thin layer chromatography (TLC) with surface-enhanced resonance Raman scattering (SERRS). TLC was used to separate the azo reaction products to confirm the component spot of azo compound, then the spot of azo compound mixed with silver sol on the TLC plate was qualitatively detected by SERRS. The limit of detection (LOD) of the method is as low as 0.50 ppm for NMA. The influence of sample matrix about the TLC-SERRS detection of NMA was investigated by experiment of simulated positive sample, and the NMA in infant pacifiers exposed to silica gel products was detected. The method of TLC-SERRS for the determination of NMA in infant pacifiers prepared with food contact silicone materials was established, and the real samples were detected. Compared with the methods ever reported, the method has the advantages of high sensitivity, specificity and low cost. It provides a new reference method for establishing a safety system for food contact silicone materials.

摘要

本研究旨在建立一种新的方法,用于测定食品接触用硅橡胶材料制备的婴儿奶嘴中 N-甲基苯胺(NMA),方法是将薄层色谱(TLC)与表面增强共振拉曼散射(SERRS)相结合,利用偶氮耦合反应进行检测。TLC 用于分离偶氮反应产物,以确认偶氮化合物的组分斑点,然后通过 SERRS 对 TLC 板上偶氮化合物与银溶胶的斑点进行定性检测。该方法对 NMA 的检测限(LOD)低至 0.50ppm。通过模拟阳性样品的实验研究了样品基质对 TLC-SERRS 检测 NMA 的影响,并检测了暴露于硅胶产品的婴儿奶嘴中的 NMA。建立了用于测定食品接触用硅橡胶材料制备的婴儿奶嘴中 NMA 的 TLC-SERRS 方法,并对实际样品进行了检测。与以往报道的方法相比,该方法具有灵敏度高、特异性强、成本低的优点。为建立食品接触用硅橡胶材料安全体系提供了新的参考方法。

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