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 (), styracin (), vanillin (), trans-cinnamic acid (), vanillic acid (), and shikimic acid (), was developed. First, eight styrax resin products (R1-R8) obtained from various tree species, which are known to contain compounds-, were extracted with a 1 : 1 mixture of supercritical CO and EtOH. Within 4 minutes, the compounds were successfully baseline separated on an Acquity UPC BEH 2-EP (3.0 × 100 mm, 1.7 µm) column using a mobile phase of supercritical CO 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 and 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.

Preparative supercritical fluid chromatography for lipid class fractionation—a novel strategy in high-resolution mass spectrometry based lipidomics

“…As a major advantage, the follow-up characterization or simply the use of the lipid class fractions obtained by prep-SFC was straightforward requiring no additional sample preparation steps as only volatile modifiers and salt additives were involved. Compared with other preparative lipid fractionation methods such as TLC, CC, prep-HPLC, and SPE, prep-SFC is fast, cost-efficient, less laborious, environmentally friendly [51], and has additional upscaling potential. In this work, up to 300 μL volumes could be injected containing 10 mg mL −1 dry lipid extract, which is 3 mg dry lipid extract compared with 0.5 μg lipid dry mass sample intake in analytical SFC (0.5 mg mL −1 , 1 μL) [14].…”

Lanostane Triterpenes from Gloeophyllum odoratum and Their Anti-Influenza Effects

“…Flash chromatography was performed on an Interchim puriFlash 4250 system, equipped with an ELSD and a PDA detector. Semi-preparative SFC was performed on a Waters Prep-15 System as described previously [27]. A Waters Viridis BEH column (5 µm; 10 × 250 mm) served as stationary phase.…”

Supercritical Fluid Chromatography in Natural Product Analysis – An Update

“…Recently, a supercritical based protocol for the extraction, analysis, and isolation of six polar compounds (o-vanillin, styracin, vanillin, trans-cinnamic acid, vanillic acid, and shikimic acid) from Styrax, an exudate from various Liquidambar trees, has been published [61]. A mixture of supercritical CO 2 and ethanol (1 : 1) was used for the extraction.…”