Department of Analytical Chemistry, University of the Basque Country UPV/EHU, Barrio Sarriena, 48940, Leioa, Biscay, Spain.
Research Centre for Experimental Marine Biology and Biotechnology (PIE), University of the Basque Country (UPV/ EHU), Plentzia, Basque Country, Spain.
Anal Bioanal Chem. 2019 Oct;411(25):6711-6722. doi: 10.1007/s00216-019-02044-1. Epub 2019 Aug 1.
The detection of organic residues that remain absorbed into the pores of ceramic artifacts constitutes a source of information regarding their management. Taking into account the poor conservation state of the potteries and the low amount of the organic tracers together with the main drawbacks to get the relevant information concerning different aspects of past societies, the detection of organic biomarkers is still an analytical challenge. In this work, an improved analytical methodology to maximize the recovery of organic markers related to wine in archeological ceramics is presented. The developed method consists on the extraction of wine-related organic compounds including tartaric acid, malic acid, fumaric acid, succinic acid, citric acid, and syringic acid by means of ultrasonic probe-assisted extraction (UPAE) followed by a preconcentration step by mixed-mode strong anion exchange and reversed-phase solid-phase extraction (SPE) and a derivatization step prior to analysis by means of gas chromatography-mass spectrometry (GC-MS). Finally, the method was applied to real archeological ceramic fragments (two dolia), suspected to have been used to store wine, together with organic residues found inside two amphorae from Zaragoza (Spain). Graphical abstract.
检测仍然被吸收到陶瓷制品孔隙中的有机残留物是了解其管理情况的一个信息来源。考虑到陶器保存状态不佳，以及有机示踪剂的含量较低，再加上获取有关过去社会不同方面相关信息的主要缺点，检测有机生物标志物仍然是一个分析挑战。在这项工作中，提出了一种改进的分析方法，以最大限度地回收与考古陶瓷中葡萄酒相关的有机标志物。所开发的方法包括通过超声探针辅助提取（UAPE）提取与葡萄酒相关的有机化合物，包括酒石酸、苹果酸、富马酸、琥珀酸、柠檬酸和丁香酸，然后通过混合模式强阴离子交换和反相固相萃取（SPE）进行浓缩步骤，以及在通过气相色谱-质谱（GC-MS）分析之前进行衍生化步骤。最后，该方法应用于两个疑似用于储存葡萄酒的真正考古陶瓷碎片（两个双耳瓶），以及在西班牙萨拉戈萨的两个双耳瓶中发现的有机残留物。
