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Comparison of extraction methods for the analysis of natural dyes in historical textiles by high-performance liquid chromatography

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An Erratum to this article was published on 24 February 2010

Abstract

Different methods for the extraction of Dactylopius coccus Costa, Rubia tinctorum L., Isatis tinctoria L., Reseda luteola L., Curcuma longa L. and Cotinus coggygria Scop. from wool fibres are investigated using high-performance liquid chromatography with diode array detector (HPLC-DAD). The efficiencies of five extraction methods which include the use of HCl (widely used extraction method), citric acid, oxalic acid, TFA and a combination of HCOOH and EDTA are compared on the basis of the (a) number, (b) relative quantities, measured as HPLC peak areas and (c) signal-to-noise ratios (S/N) of the compounds extracted from the wool substrates. Flavonoid glycosides and curcuminoids contained in R. luteola L. and C. longa L., respectively, according to liquid chromatography with mass spectrometry (LC-MS) identifications, are not detected after treating the fibres with HCl. All the other milder methods are successful in extracting these compounds. Experiments are performed using HPLC-DAD to compare the HPLC peak areas and the S/N of the following extracted compounds: indigotin, indirubin, curcumin, demethoxycurcumin, bisdemethoxycurcumin, fisetin, sulfuretin, luteolin, luteolin-7-O-glucoside, apigenin, carminic acid, alizarin, puruprin and rubiadin. It is shown that the TFA method provides overall the best results as it gives elevated extraction yields except for fisetin, luteolin, apigenin and luteolin-7-O-glucoside and highest S/N except for fisetin and luteolin-7-O-glucoside. It is noteworthy that treatment of the fibres with the typical HCl extraction method results overall in very low S/N. The TFA method is selected for further studies, as follows. First, it is applied on silk dyed samples and compared with the HCl method. The same relative differences of the TFA and HCl methods observed for the wool dyed samples are reported for the silk dyed samples too, except for rubiadin, luteolin and apigenin. Thus, in most cases, the nature of the substrate (wool or silk) appears to have negligible effects on the relative difference of the two extraction methods. Second, the selected TFA method is applied to treat wool and silk historical samples extracted from textiles of the Mamluk period, resulting in the identification of several colouring compounds. In all extraction methods mentioned above, DMSO is used to dissolve the dyes, after acid treatment.

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Acknowledgements

The authors would like to thank M. van Bommel for his critical review and comments and M. Sardi and A. Ozolin for providing the historical samples. Support by the General Secreteriat for Research and Technology of Greece (Programme PENED 2003-697) and the Getty Foundation (USA) is gratefully acknowledged.

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Authors and Affiliations

  1. Ormylia Art Diagnosis Center, Ormylia, 63071, Chalkidiki, Greece

    Lemonia Valianou & Ioannis Karapanagiotis

  2. School of Chemical Engineering, National Technical University of Athens, Athens, 15773, Greece

    Lemonia Valianou & Yannis Chryssoulakis

Authors
  1. Lemonia Valianou
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  2. Ioannis Karapanagiotis
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  3. Yannis Chryssoulakis
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Correspondence to Ioannis Karapanagiotis.

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An erratum to this article can be found at http://dx.doi.org/10.1007/s00216-010-3528-8

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Valianou, L., Karapanagiotis, I. & Chryssoulakis, Y. Comparison of extraction methods for the analysis of natural dyes in historical textiles by high-performance liquid chromatography. Anal Bioanal Chem 395, 2175–2189 (2009). https://doi.org/10.1007/s00216-009-3137-6

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  • DOI: https://doi.org/10.1007/s00216-009-3137-6

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