Abstract

Detailed knowledge on natural dyes is important for agronomy and quality control as well as the fastness, stability, and analysis of dyed textiles. Weld (Reseda luteola L.), which is a source of flavone-based yellow dye, is the focus of this study. One aim was to reduce the required amount of dyed textile to ≤50 μg for a successful chromatographic analysis. The second aim was to unambiguously confirm the identity of all weld flavones. By carrying out the extraction of 50 μg dyed wool with 25 μL of solvent and analysis by reversed-phase UHPLC at 345 nm, reproducible chromatographic fingerprints could be obtained with good signal to noise ratios. Ten baseline separated peaks with relative areas ≥1% were separated in 6 min. Through repeated polyamide column chromatography and prepHPLC, the compounds corresponding with the fingerprint peaks were purified from dried weld. Each was unequivocally identified, including the position and configuration of attached sugars, by means of 1D and 2D NMR and high-resolution MS. Apigenin-4′-O-glucoside and luteolin-4′-O-glucoside were additionally identified as two trace flavones co-eluting with other flavone glucosides, the former for the first time in weld. The microextraction might be extended to other used dye plants, thus reducing the required amount of precious historical textiles.

Highlights

  • Since the stone age, mankind has dyed his clothes for decoration

  • Earlier we have shown that by using short UHPLC columns for dye substances significant time reduction and sensitivity gains are possible [30]

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Summary

Introduction

Mankind has dyed his clothes for decoration. Later rugs and tapestries were dyed. To facilitate the re-introduction of natural dyes, over the last 25 years many papers have appeared, for instance on screening methods for agronomic studies of dye plants [2,3], the fastness of dyed textiles [4], the colorimetric properties of dye plants and their individual constituents [5], mild extraction methods for textiles [6,7,8], degradation of dyes [9,10,11], safety of natural dyes [12], the development of new production routes [13], and analysis of dyed textiles [1,14] Concerning the latter topic, natural dye analysis is of great importance for historians and conservators. It can help to shed light on previous restorations and help future restorations [1]

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