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首页> 外文期刊>International journal of mass spectrometry >Analysis of archaeological triacylglycerols by high resolution nanoESI, FT-ICR MS and IRMPD MS/MS: Application to 5th century BC-4th century AD oil lamps from Olbia (Ukraine)
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Analysis of archaeological triacylglycerols by high resolution nanoESI, FT-ICR MS and IRMPD MS/MS: Application to 5th century BC-4th century AD oil lamps from Olbia (Ukraine)

机译：通过高分辨率nanoESI，FT-ICR MS和IRMPD MS / MS分析考古三酰甘油：应用于奥尔比亚（乌克兰）的5世纪BC-4世纪AD油灯

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摘要

This work presents the precise identification of triacylglycerols (TAGs) extracted from archaeological samples using a methodology based on nanoelectrospray and Fourier transform mass spectrometry. The archaeological TAG identification needs adapted sample preparation protocols to trace samples in advanced degradation state. More precisely, the proposed preparation procedure includes extraction of the lipid components from finely grinded ceramic using dichloromethane/methanol mixture with additional ultrasonication treatment, and TAG purification by solid phase extraction on a diol cartridge. Focusing on the analytical approach, the implementation of "in-house" species-dependent TAG database was investigated using MS and InfraRed Multiphoton Dissociation (IRMPD) MS/MS spectra; several vegetal oils, dairy products and animal fats were studied. The high mass accuracy of the Fourier transform analyzer (m below 2.5 ppm) provides easier data interpretation, and allows distinction between products of different origins. In details, the IRMPD spectra of the lithiated TAGs reveal fragmentation reactions including loss of free neutral fatty acid and loss of fatty acid as alpha,beta-unsaturated moieties. Based on the developed preparation procedure and on the constituted database, TAG extracts from 5th century BC to 4th century AD Olbia lamps were analyzed. The structural information obtained succeeds in identifying that bovine/ovine fats were used as fuel used in these archaeological Olbia lamps. (C) 2009 Elsevier B.V. All rights reserved.
机译：这项工作提出了使用基于纳米电喷雾和傅立叶变换质谱的方法从考古样品中提取的三酰基甘油（TAG）的精确鉴定。考古TAG识别需要适应性的样品制备方案，以追踪处于高级降解状态的样品。更准确地说，拟议的制备程序包括使用二氯甲烷/甲醇混合物和额外的超声处理从精细研磨的陶瓷中提取脂质成分，以及通过在二醇盒上进行固相提取进行TAG纯化。着重于分析方法，使用MS和红外多光子离解（IRMPD）MS / MS光谱研究了“内部”物种相关TAG数据库的实现;研究了几种植物油，乳制品和动物脂肪。傅立叶变换分析仪的高质量精度（低于2.5 ppm的m）提供了更容易的数据解释，并且可以区分不同来源的产品。详细地，锂化TAG的IRMPD光谱揭示了片段化反应，包括游离的中性脂肪酸的损失和作为α，β-不饱和部分的脂肪酸的损失。根据制定的制备程序和所建立的数据库，分析了公元前5世纪至公元4世纪的奥尔比亚灯的TAG提取物。获得的结构信息成功地确定了牛/羊脂肪被用作这些考古奥尔比亚灯中使用的燃料。 （C）2009 Elsevier B.V.保留所有权利。

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