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  • TLC and HPTLC‐APCI‐MS for t...
    Schendzielorz, Marcel; Schmidt, Theresa; Puchalla, Nils; Csuk, René; Kramell, Annemarie E.

    Phytochemical analysis, January 2024, 2024-Jan, 2024-01-00, 20240101, Letnik: 35, Številka: 1
    Journal Article

    Introduction Depending on their terpenoid and phenolic constituents plant resins can be classified as diterpenoid, triterpenoid or phenolic resins; thereby the profile of diterpenes and triterpenes is considered as genus‐ or even species‐specific. Objectives We aimed to develop a simple, rapid, inexpensive, sensitive and specific method for the identification of resin‐specific triterpenoid and phenolic compounds in plant resins using (HP)TLC (high‐performance) thin‐layer chromatography combined with APCI‐MS (atmospheric pressure chemical ionisation mass spectrometry) and post‐chromatographic detection reactions. Methods Twenty resin samples from different plant species were analysed. Different extraction procedures, post‐chromatographic detection reagents as well as various sorbents and solvents for planar chromatography were tested. To evaluate the potential of the optimised (HP)TLC‐APCI‐MS methods, parameter such as limit of detection (LOD) was determined for selected marker compounds. Results Our protocol enabled qualitative analyses of chemotaxonomic molecular markers in natural resins such as dammar, mastic, olibanum and benzoin. For the first time, the application of thionyl chloride‐stannic chloride reagent for a specific post‐chromatographic detection of triterpenes is reported, sometimes even allowing discrimination between isomers based on their characteristic colour sequences. For triterpene acids, triterpene alcohols and phenolic compounds, detection limits of 2–20 ng/TLC zone and a system precision with a relative standard deviation (RSD) in the range of 3.9%–7.0% were achieved by (HP)TLC‐APCI‐MS. The applicability of the method for the analysis of resin‐based varnishes was successfully tested on a mastic‐based varnish. Thus, the method we propose is a helpful tool for the discrimination of resins and resin‐based varnishes with respect to their botanical origin. In this study, we developed a simple, rapid, cost‐effective, sensitive and specific method for the identification of chemotaxonomic molecular markers in plant resins such as dammar, mastic, olibanum and benzoin using (HP)TLC combined with APCI‐MS and post‐chromatographic detection reactions. For the first time, the application of thionyl chloride‐stannic chloride reagent for a specific post‐chromatographic detection of triterpenes is reported, sometimes even allowing discrimination between isomers based on their characteristic color sequences.