title: Fast and Green - CO2 Based Extraction, Isolation, and Quantification of Phenolic Styrax Constituents.
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 variousLiquidambartree species, which are known to contain compounds2-6, were extracted with a 1 : 1 mixture of supercritical CO2and EtOH. Within 4 minutes, the compounds were successfully baseline separated on an Acquity UPC2BEH 2-EP (3.0 × 100 mm, 1.7 µm) column using a mobile phase of supercritical CO2and 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 constituents2and4from 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.
authors.affiliation: Department of Pharmacognosy, University of Vienna, Vienna, Austria.
authors.forename: Johanna
authors.initials: J
authors.lastname: Scheuba
authors.affiliation: Department of Pharmacognosy, University of Vienna, Vienna, Austria.
authors.forename: Valerie-Katharina
authors.initials: VK
authors.lastname: Wronski
authors.affiliation: Department of Pharmacognosy, University of Vienna, Vienna, Austria.
authors.forename: Judith M
authors.initials: JM
authors.lastname: Rollinger
authors.affiliation: Department of Pharmacognosy, University of Vienna, Vienna, Austria.
authors.forename: Ulrike
authors.initials: U
authors.lastname: Grienke
mesh_terms: D002245:Carbon Dioxide; D025924:Chromatography, Supercritical Fluid / Q000379:methods*; D000432:Methanol; D010636:Phenols / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification; D012116:Resins, Plant / Q000737:chemistry*; D032362:Styrax / Q000737:chemistry*
chemical_list: D010636:Phenols; D012116:Resins, Plant; D002245:Carbon Dioxide; D000432:Methanol