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The possibilities and limitations of supercritical fluid extraction of natural products of low, medium and high polarity under very high pressure and with polar modifiers has been investigated. The medicinal herbs marigold (Calendula officinalis), hawthorn (Crataegus sp.) and chamomile (Matricaria recutita) were used as models in this study. Extraction profiles and the spectra of extractable metabolites were recorded following extraction with mixtures of carbon dioxide:ethanol of varying proportions (0-20% ethanol) and at various pressures in the range 300-689 bar. Components were identified by HPLC-PAD-MS or GC-MS and quantified by HPLC or GC as appropriate. Extraction yields under the varying conditions depended to a large extent on the profiles of secondary metabolites present in the three drugs. Whereas the extractability of lipophilic compounds increased substantially at pressures above 300 bar, the yields of polyphenolic and glycosidic compounds remained low even at 689 bar and with 20% modifier in the extraction fluid.

The effects of pressure and co-solvent on the extraction of anti-inflammatory faradiol esters in marigold (Calendula officinalis L.) were investigated by supercritical fluid extraction at laboratory and pilot scales. Pressures higher than 300 bar and modifier (ethanol) concentrations ranging from 0 to 20% (v/v) were used at an extraction temperature of 50 degrees C. With an analytical extractor, exhaustive extraction of the drug and highest concentrations in the extracts were achieved with 0.5% ethanol at the maximum pressure of 689 bar. Increased modifier concentrations improved the extractability at lower pressure, but the higher amount of total extractables led to a lower concentration of faradiol esters in the extracts. The HPLC fingerprints of the extracts, the yields of total extract and the concentration of faradiol esters obtained with analytical and pilot scale extractors under the same conditions were comparable.

An efficient protocol for the preparative purification of the major tea catechins (-)-epicatechin gallate (3) and epigallocatechin gallate (5) has been developed, employing liquid-liquid partitioning, high-speed countercurrent chromatography, and gel chromatography for final purification. The method is suitable for scale-up to significantly larger quantities.

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