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Identification of natural indigo in historical textiles by GC–MS

Analytical and Bioanalytical Chemistry volume 407, pages 1695–1704 (2015)Cite this article

Abstract

The possibility of successfully applying a common GC–MS procedure for identification in one step of all types of dyes from plants of unknown origin and from historical objects is particularly attractive due to the high separation efficiency of the capillary columns, the MS detection sensitivity and the reproducibility of results. In this work, GC–MS analysis, previously and successfully used for the characterization of anthraquinones, flavonoids and tannins from plant extracts and historical samples, has been tested on indigoid dyestuffs. An analytical procedure based on the silylating agent N,O-bis-(trimethylsilyl)trifluoroacetamide (BSTFA) with 1 % trimethylchlorosilane (TMCS) was applied to pure molecules of indigotin and indirubin and to plant extracts of Indigofera tinctoria L. and Isatis tinctoria L. Preliminary tests have been done to establish the chromatographic conditions and the derivatization amounts most suitable for the simultaneous detection of indigoid molecules and of the other natural compounds, such as fatty acids, carboxylic acids and sugars, contained within the plant extracts. In order to assess the capacity and the sensitivity of the analytical procedure in typical archaeometric applications, wool samples dyed in the laboratory with indigo were analysed by mimicking the sample amounts typically available with historical objects. The electron ionization (EI) spectra of the main silylated derivatives of indigoid molecules obtained in this way constitute the necessary data set for the characterization of natural extracts and historical works of art. Subsequently, the procedure has been applied to historical samples for the detection of indigo and of other dyestuffs eventually contained in samples. Additional information, useful for restoration and preservation of works of art, could be also obtained on the nature of stains and smudges present on the sampled textile material. The GC–MS method turns out to be an efficient and fast analytical tool also for the identification of natural indigo in plants and textile artefacts, providing results complementary to those from high-performance liquid chromatography (HPLC).

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Acknowledgments

CRITT Horticole (Rochefort sur Mer, France) is gratefully acknowledged for supplying the plant extracts. This work has been partially supported through the PRIN 2010-2011 (MIUR, Italy) project: Sustainability in cultural heritage: from diagnosis to the development of innovative systems for consolidation, cleaning and protection.

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  1. Dipartimento di Chimica, Universita di Torino, Via Giuria 7, 10125, Turin, Italy

    Laura Degani, Chiara Riedo & Oscar Chiantore

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  1. Laura Degani
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  2. Chiara Riedo
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  3. Oscar Chiantore
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Correspondence to Oscar Chiantore.

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Degani, L., Riedo, C. & Chiantore, O. Identification of natural indigo in historical textiles by GC–MS. Anal Bioanal Chem 407, 1695–1704 (2015). https://doi.org/10.1007/s00216-014-8423-2

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  • DOI: https://doi.org/10.1007/s00216-014-8423-2

Keywords

  • Natural indigo
  • GC–MS
  • Historical textiles
  • Archaeometry fine arts