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Planta Med 2017; 83(12/13): 1068-1075
DOI: 10.1055/s-0043-105499
Natural Product Chemistry and Analytical Studies
Original Papers
Georg Thieme Verlag KG Stuttgart · New York

Fast and Green – CO2 Based Extraction, Isolation, and Quantification of Phenolic Styrax Constituents[*]

Johanna Scheuba
Department of Pharmacognosy, University of Vienna, Vienna, Austria
,
Valerie-Katharina Wronski
Department of Pharmacognosy, University of Vienna, Vienna, Austria
,
Judith M. Rollinger
Department of Pharmacognosy, University of Vienna, Vienna, Austria
,
Ulrike Grienke
Department of Pharmacognosy, University of Vienna, Vienna, Austria
› Author Affiliations
Further Information

Publication History

received 25 January 2017
revised 23 February 2017

accepted 04 March 2017

Publication Date:
16 March 2017 (online)

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Abstract

In this study the first supercritical fluid based protocol for the extraction, analysis, and isolation of six polar compounds, i.e., o-vanillin (1), styracin (2), vanillin (3), trans-cinnamic acid (4), vanillic acid (5), and shikimic acid (6), was developed. First, eight styrax resin products (R1–R8) obtained from various Liquidambar tree species, which are known to contain compounds 2–6, were extracted with a 1 : 1 mixture of supercritical CO2 and EtOH. Within 4 minutes, the compounds were successfully baseline separated on an Acquity UPC2 BEH 2-EP (3.0 × 100 mm, 1.7 µm) column using a mobile phase of supercritical CO2 and MeOH with 0.1 % phosphoric acid. The compounds were quantified and the method was validated according to current ICH guidelines. Scaling up to preparative supercritical fluid chromatography using a Viridis BEH 2-EP (10 × 250 mm, 5 µm) column allowed for a fast separation and isolation of the selected constituents 2 and 4 from R6 within 7 minutes. This supercritical fluid protocol is easily adaptable to compounds of similar polarity. The increase in speed and its environmental friendliness underline its superiority over conventional set-ups.

Key words

Liquidambar orientalis - Hamamelidaceae - supercritical fluid extraction - supercritical fluid chromatography - ultra-performance convergence chromatography - styrax

* Dedicated to Professor Dr. Max Wichtl in recognition of his outstanding contribution to pharmacognosy research.


Supporting Information

Chromatograms (UPC2) showing the method development and the eight resin products (R1–R8) with optimised parameters, as well as chromatograms (HPLC) of isolated pure compounds 2 and 4 including relevant mass spectra are available as Supporting Information.

 

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