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用于表面增强拉曼光谱法鉴定蒽醌染料的样品处理优化

Optimization of sample treatment for the identification of anthraquinone dyes by surface-enhanced Raman spectroscopy.

作者信息

Marcaida Iker, Maguregui Maite, Morillas Héctor, García-Florentino Cristina, Pintus Valentina, Aguayo Tomás, Campos-Vallette Marcelo, Madariaga Juan Manuel

机构信息

Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country UPV/EHU, P.O. Box 644, 48080, Bilbao, Basque Country, Spain.

Department of Analytical Chemistry, Faculty of Pharmacy, University of the Basque Country UPV/EHU, P.O. Box 450, 01080, Vitoria-Gasteiz, Basque Country, Spain.

出版信息

Anal Bioanal Chem. 2017 Mar;409(8):2221-2228. doi: 10.1007/s00216-016-0169-6. Epub 2017 Jan 13.

Abstract

The study and characterization of old artifacts such as pigments requires the use of techniques that need a small amount of sample to perform the analysis because of the high value of these samples. In recent years, organic molecules such as anthraquinone dyes have been identified by surface-enhanced Raman spectroscopy (SERS). However, different sample treatments must be applied to isolate the organic dye from the mordant, which produces great fluorescence in the Raman measurements. In this work, optimization of sample treatment for the SERS analysis of anthraquinone dyes was performed. Sample mass, the organic solvent, and its volume were optimized and different slide materials and excitation lasers were compared to choose the best conditions for the identification of the dyes. The optimization of sample treatment resulted in 5 mg of sample as the optimum amount. Further, two consecutive extractions with 0.5 mL of ethyl acetate was the best option for the extraction of the dye. A quartz slide was used instead of a glass slide to reduce background signal, and an excitation laser of 532 nm offers better results than one of 785 nm. The optimized method was applied to the characterization of the dyes used in Pompeian pink and purple lake pigments. Alizarin and purpurin anthraquinone dyes, obtained from madder lake, were identified as the organic colorants. The SERS results were confirmed by those obtained by means of UV-visible spectroscopy. Graphical Abstract ᅟ.

摘要

对颜料等古老文物的研究和表征需要使用一些技术,由于这些样品价值高昂,分析时只需少量样品。近年来,通过表面增强拉曼光谱(SERS)已鉴定出蒽醌染料等有机分子。然而,必须采用不同的样品处理方法,以便从媒染剂中分离出有机染料,媒染剂在拉曼测量中会产生很强的荧光。在这项工作中,对用于蒽醌染料SERS分析的样品处理进行了优化。对样品质量、有机溶剂及其体积进行了优化,并比较了不同的载玻片材料和激发激光,以选择鉴定染料的最佳条件。样品处理的优化结果表明,5mg样品为最佳用量。此外,用0.5mL乙酸乙酯连续萃取两次是提取染料的最佳选择。使用石英载玻片代替玻璃载玻片以降低背景信号,532nm的激发激光比785nm的激发激光能提供更好的结果。该优化方法应用于庞贝粉红和紫色湖颜料中所用染料的表征。从茜草湖中获得的茜素和紫茜素蒽醌染料被鉴定为有机色素。SERS结果通过紫外可见光谱法得到的结果得到了证实。图形摘要ᅟ。

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