Abstract
Headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) have traditionally been used, in combination with other analyses, for the chemical characterization of organic residues recovered from archaeological specimens. Recently in many life science fields, comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) has provided numerous benefits over GC-MS. This study represents the first use of HS-SPME-GC×GC-TOFMS to characterize specimens from an experimental modern reference collection. Solvent extractions and direct analyses were performed on materials such as ivory, bone, antlers, animal tissue, human tissue, sediment, and resin. Thicker film column sets were preferred due to reduced column overloading. The samples analyzed by HS-SPME directly on a specimen appeared to give unique signatures and generally produced a higher response than for the solvent-extracted residues. A non-destructive screening approach of specimens may, therefore, be possible. Resin and beeswax mixtures prepared by heating for different lengths of time appeared to provide distinctly different volatile signatures, suggesting that GC×GC-TOFMS may be capable of differentiating alterations to resin in future studies. Further development of GC×GC-TOFMS methods for archaeological applications will provide a valuable tool to uncover significant information on prehistoric technological changes and cultural behavior.
Highlights
Gas chromatography coupled to mass spectrometry (GC-MS), in combination with non-contact sampling methods such as headspace solid-phase microextraction (HS-SPME), is a popular technique used in archaeological research for organic residue analyses [1,2,3,4,5]
It is proposed that characterization of archaeological samples would benefit substantially from the use of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GCGC-TOFMS)
Additional studies need to be performed to answer this question in its entirety, this sample was analyzed in order to incorporate a particular situation in which GCGC-TOFMS may be useful for providing information to differentiate two volatile signatures
Summary
Gas chromatography coupled to mass spectrometry (GC-MS), in combination with non-contact sampling methods such as headspace solid-phase microextraction (HS-SPME), is a popular technique used in archaeological research for organic residue analyses [1,2,3,4,5]. It is proposed that characterization of archaeological samples would benefit substantially from the use of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GCGC-TOFMS) This comprehensive, multidimensional technique offers an improved peak capacity, leading to considerable enhancement in peak separation and subsequent quantification. The output based on three axes (1 tR , 2 tR , and intensity) improves the visualization of the characteristics of complex samples, presenting an attractive option for end users in various life science application areas [16] This is further enhanced by the availability of a fourth mass spectral axis that provides information about the identity of the chromatographic signals through the use of deconvoluted TOFMS fragmentation spectra that can be compared to reference spectral libraries. This was done with the aim of presenting insights into the use of GCGC-TOFMS in the future of archaeological research
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