Archaeometric Data from Mass Spectrometric Analysis of Organic Materials: Proteins, Lipids, Terpenoid Resins, Lignocellulosic Polymers, and Dyestuff

Colombini, Maria Perla; Modugno, Francesca; Ribechini, Erika

doi:10.1002/9781118180730.ch36

Cited by 8 publications

(12 citation statements)

References 165 publications

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“…The resin acids oleanonic acid, moronic acid, and the isomers masticadienonic and isomasticadienonic acid are markers for resin from Pistacia sp. , although oleanonic acid is also found in other plant resins so is not itself diagnostic ( 36 – 38 ). Peaks for moronic acid were very low in scan mode and usually only detectable in SIM mode at a retention time determined by running reference samples.…”

Section: Resultsmentioning

confidence: 99%

“…The detector was an Agilent 5975 mass spectrometer using EI at 70 eV. Each sample was analyzed twice, first in scan mode over the range 50 to 750 amu, then in SIM mode targeting different ions over three time periods: 0 to 15 min (aromatics) m / z 105, 205, 267, and 297 ( 49 ); 15 to 25 min for conifer resin, pitch, and bitumen m / z 219, 239, 253, 459, 191, and 217 ( 30 – 32 , 40 ); and 25 to 35 mins for Pistacia resin and bitumen m / z 189, 409, 421, 526, 191, and 217 ( 36 , 40 ).…”

Section: Methodsmentioning

confidence: 99%

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Molecular analysis of black coatings and anointing fluids from ancient Egyptian coffins, mummy cases, and funerary objects

Fulcher

Serpico

Taylor

et al. 2021

Proc. Natl. Acad. Sci. U.S.A.

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Black organic coatings and ritual deposits on ancient Egyptian coffins and cartonnage cases are important and understudied sources of evidence about the rituals of funerary practice. Sometimes, the coatings were applied extensively over the surface of the coffin, resembling paint; in other cases, they were poured over the mummy case or wrapped body, presumably as part of a funerary ritual. For this study, multiple samples of black coatings and ritual liquids were taken from 20 Egyptian funerary items dating to a specific time period (c. 943 to 716 BC). Multiple sampling from each object enabled several comparisons to be made: the variability of the black coating within one application, the variability between two applications on one object, and the variability from object to object. All samples were analyzed for lipids using gas chromatography–mass spectrometry (GC-MS), and 51 samples from across the 20 items were further analyzed for the presence of bitumen using solid phase separation followed by selected ion monitoring GC-MS. The majority of the black substances were found to comprise a complex mixture of organic materials, including bitumen from the Dead Sea, conifer resin, and Pistacia resin, providing evidence for a continuation in international trade between Egypt and the eastern Mediterranean after the Late Bronze Age. Both the coating and the anointing liquid are very similar to mummification balms, pointing to parallels with Egyptian embalming rituals and raising questions about the practical aspects of Egyptian funerary practice.

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Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Molecular analysis of black coatings and anointing fluids from ancient Egyptian coffins, mummy cases, and funerary objects

Fulcher

Serpico

Taylor

et al. 2021

Proc. Natl. Acad. Sci. U.S.A.

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“…Such analytical approaches use bulk analysis to examine ambers and to obtain information on the botanical origins of archaeological findings. In addition, due to the high molecular weight/polymeric nature of ambers, some researchers have used analytical pyrolysis coupled with GC/MS systems (Py-GC/MS) [1,2,5,[20][21][22][23]. When analytical pyrolysis is used, the chemical composition of the sample is reconstructed on the basis of an interpretation of the molecular profile of the thermal degradation products of the original components, and on the recognition of specific molecular markers or molecular patterns, which give characteristic fingerprints of the pyrolysed material.…”

Section: Introductionmentioning

confidence: 99%

“…Tetramethyl ammonium hydroxide (TMAH) allows hydrolysis and methylation to be obtained simultaneously and is thus widely used derivatisation reagent [1,20]. Recently, silylating reactions using hexamethyldisilazane (HMDS) have been proposed as an alternative in the analysis of ambers [21,23,25]. HMDS proved its potential with respect to the strongly alkaline TMAH reagent.…”

Section: Introductionmentioning

confidence: 99%

Analytical pyrolysis with in-situ silylation, Py(HMDS)-GC/MS, for the chemical characterization of archaeological and historical amber objects

et al. 2013

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Introduction: An optimised analytical technique based on pyrolysis coupled with gas chromatography/mass spectrometry (Py-GC/MS) and derivatisation in situ with hexamethyldisilazane (HMDS) was used to study several archaeological and artistic amber objects. The aim was to verify the authenticity of the objects and to provide historical information regarding the geographical origin of the ambers, and thus reveal the trade routes between different ancient civilizations. Results: Py-GC/MS using HMDS as a silylating agent enabled us not only to identify the geographical origin of the archaeological and artistic ambers as succinites, but also highlighted the degradation of amber objects revealing a lower abundance of free diterpenes on the surface. Conclusion: This work demonstrates the capability of Py-GC/MS with silylation in situ to identify the geographical origin of archaeological ambers and to provide crucial information regarding their degradation process. The porous and rough appearance of the outer layer can be correlated with the higher lixiviation and to the evaporation of free diterpenes from the surface. The knowledge of the amber degradation mechanisms is crucial to select proper conservation-restoration methods.

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“…In the last few years, laser‐based ionization techniques, e.g. laser desorption/ionization (LDI), graphite‐assisted LDI and matrix‐assisted LDI (MALDI), have become popular and useful for mass spectrometric analyses of organic materials in the Cultural Heritage . These techniques require negligible sample manipulation and no sample pre‐treatment.…”

Section: Introductionmentioning

confidence: 99%

Positive and negative‐mode laser desorption/ionization‐mass spectrometry (LDI‐MS) for the detection of indigoids in archaeological purple

2013

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Laser-based ionization techniques have demonstrated to be a valuable analytical tool to study organic pigments by mass spectrometric analyses. Though laser-based ionization techniques have identified several natural and synthetic organic dyes and pigments, they have never been used in the characterization of purple. In this work, positive and negative-mode laser desorption/ionization mass spectrometry (LDI-MS) was used for the first time to detect indigoids in shellfish purple. The method was used to study organic residues collected from archaeological ceramic fragments that were known to contain purple, as determined by a classical high-performance liquid chromatography-based procedure. LDI-MS provides a mass spectral fingerprint of shellfish purple, and it was found to be a rapid and successful tool for the identification of purple. In addition, a comparison between positive and negative mode ionization highlighted the complementarity of the two ionization modes. On the one hand, the negative-ion mode LDI-MS showed a better selectivity and sensitivity to brominated molecules, such as 6,6'-dibromoindigo, 6-monobromoindigo, 6,6'-dibromoindirubin, 6- and 6'-monobromoindirubin, thanks to their electronegativity, and produced simpler mass spectra. On the other hand, negative-ion mode LDI-MS was found to have a lower sensitivity to non-brominated compounds, such as indigo and indirubin, whose presence can be established in any case by collecting the complementary positive-ion LDI mass spectrum.

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Archaeometric Data from Mass Spectrometric Analysis of Organic Materials: Proteins, Lipids, Terpenoid Resins, Lignocellulosic Polymers, and Dyestuff

Cited by 8 publications

References 165 publications

Molecular analysis of black coatings and anointing fluids from ancient Egyptian coffins, mummy cases, and funerary objects

Molecular analysis of black coatings and anointing fluids from ancient Egyptian coffins, mummy cases, and funerary objects

Analytical pyrolysis with in-situ silylation, Py(HMDS)-GC/MS, for the chemical characterization of archaeological and historical amber objects

Positive and negative‐mode laser desorption/ionization‐mass spectrometry (LDI‐MS) for the detection of indigoids in archaeological purple

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