An alternative analytical method based on ultrasound micro bath hydrolysis and GC-MS analysis for the characterization of organic biomarkers in archaeological ceramics.
The analysis of organic biomarkers in ancient and valuable archaeological remains provides a worthwhile source of information regarding their management. This work was focused on the development of an analytical procedure to characterize organic residues that have remained in archaeological ceramic samples. A novel analytical approach based on an alkaline hydrolysis by means of an ultrasound micro bath followed by liquid extraction was proposed to isolate saturated and unsaturated fatty acids, degradation products such as dihydroxy acids or dienoic fatty acids, isoprenoid fatty acids, and many other biomarkers from archaeological remains. This main goal has been achieved after the optimization of the main parameters affecting the hydrolysis step, the extraction procedure, and the derivatization step prior to the gas chromatography-mass spectrometry analysis. In this work, archaeological ceramic remains suspected to have been used by Basque Whalers to store whale oil in the period from the sixteenth to the seventeenth century were studied. Nevertheless, the proposed method is useful to determine the organic remains preserved in many other archaeological ceramic remains. Moreover, this methodology can be used to determine organic remains in any porous ceramic, archaeological or not. The preliminary results of the analysis of ceramic vessels led to the determination of some interesting unsaturated compounds such as 11-eicosenoic acid, an important biomarker of marine commodities, and several saturated fatty acids, which could be indicative of having used the vessels to store whale oil. Graphical abstract ᅟ.
Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, Spain. laura.blanco@ehu.eus.
Laura
L
Blanco-Zubiaguirre
Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, Spain.
Maitane
M
Olivares
Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, Spain.
Kepa
K
Castro
Department of Geography, Prehistory and Archaeology, University of the Basque Country (UPV/EHU), 01006, Vitoria-Gasteiz, Araba, Spain.|IKERBASQUE, Basque Foundation for Science, Maria Diaz de Haro 3, 48013, Bilbao, Spain.
Javier G
JG
Iñañez
Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, Spain.
Juan Manuel
JM
Madariaga
D001106:Archaeology / Q000295:instrumentation / Q000379:methods*; D015415:Biomarkers / Q000032:analysis; D002516:Ceramics / Q000737:chemistry*; D003297:Cooking and Eating Utensils; D005227:Fatty Acids / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006868:Hydrolysis; D000069453:Ultrasonic Waves
D015415:Biomarkers; D005227:Fatty Acids
Archaeological organic remains; Fatty acids; Gas chromatography–mass spectrometry; Ultrasound micro bath