Lipids are the most widely studied compounds in archaeological pottery, thanks to their hydrophobicity that makes them particularly durable over time compared to other organic components [1]. However, most of the lipids are featured by reactive functional groups that fatally lead to their degradation in archaeological site, furtherly complicating the interpretations on the origin of lipid matter [2]. In-lab alteration processes such as thermal decomposition, oxidation and hydrolysis reactions have been already investigated [3]. Such ageing tests can provide key elements to study the formation of characteristic compounds and better address the origin of the organic archaeological remains. In the present study, in-lab thermo-oxidative treatments have been carried out to simulate the natural degradation of the lipid matter. In detail, standards of pure triglicerides such as triolein and trilinolein, and extra-virgin olive oil sample were kept in an oven at 120°C for three weeks. High and medium volatility components, including short-chain fatty acids, aldehydes, ketones, lactones and esters, were analyzed by using headspace solid-phase microextraction prior to gas chromatography-mass spectrometry (GC-MS), while lowvolatility and polar compounds, such as medium- and long-chain fatty acids or (α,ω)-dicarboxylic acids, were converted into trimethylsilyl ethers (TMS) derivatives and analyzed by GC-MS. The degradation of the intact lipids was monitored by using non-aqueous reversed phase high performance liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry. [1] B. Stern, C. Heron, T. Tellefsen, M. Serpico. New investigations into the Uluburun resin cargo. J. Archaeol. Sci. 35 (2008) 2188-2203. [2] M. Regert. Analytical strategies for discriminating archeological fatty substances from animal origin. Mass. Spectrom. Rev. 30 (2011) 177-220. [3] M. P. Colombini, F. Modugno, E. Ribechini. Organic mass spectrometry in archaeology: evidence for Brassicaceae seed oil in Egyptian ceramic lamps. J Mass. Spectrom. 40 (2005) 890-898.
CHARACTERIZATION OF IN-LAB AGED LIPIDS BY USING GAS AND LIQUID CHROMATOGRAPHY APPROACHES COUPLED TO MASS SPECTROMETRY
V. Chiaia
;G. Micalizzi;D. Donnarumma;A. Irto;C. Bretti;P. Cardiano;P. Q. Tranchida;L. Mondello
2022-01-01
Abstract
Lipids are the most widely studied compounds in archaeological pottery, thanks to their hydrophobicity that makes them particularly durable over time compared to other organic components [1]. However, most of the lipids are featured by reactive functional groups that fatally lead to their degradation in archaeological site, furtherly complicating the interpretations on the origin of lipid matter [2]. In-lab alteration processes such as thermal decomposition, oxidation and hydrolysis reactions have been already investigated [3]. Such ageing tests can provide key elements to study the formation of characteristic compounds and better address the origin of the organic archaeological remains. In the present study, in-lab thermo-oxidative treatments have been carried out to simulate the natural degradation of the lipid matter. In detail, standards of pure triglicerides such as triolein and trilinolein, and extra-virgin olive oil sample were kept in an oven at 120°C for three weeks. High and medium volatility components, including short-chain fatty acids, aldehydes, ketones, lactones and esters, were analyzed by using headspace solid-phase microextraction prior to gas chromatography-mass spectrometry (GC-MS), while lowvolatility and polar compounds, such as medium- and long-chain fatty acids or (α,ω)-dicarboxylic acids, were converted into trimethylsilyl ethers (TMS) derivatives and analyzed by GC-MS. The degradation of the intact lipids was monitored by using non-aqueous reversed phase high performance liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry. [1] B. Stern, C. Heron, T. Tellefsen, M. Serpico. New investigations into the Uluburun resin cargo. J. Archaeol. Sci. 35 (2008) 2188-2203. [2] M. Regert. Analytical strategies for discriminating archeological fatty substances from animal origin. Mass. Spectrom. Rev. 30 (2011) 177-220. [3] M. P. Colombini, F. Modugno, E. Ribechini. Organic mass spectrometry in archaeology: evidence for Brassicaceae seed oil in Egyptian ceramic lamps. J Mass. Spectrom. 40 (2005) 890-898.Pubblicazioni consigliate
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