Extraction and Isolation of a Natural Product from Schisandra Berry Extract Using SFE and SFC

Importance of the Topic

Schisandra chinensis berries contain valuable lignans such as schisandrin A, recognized for antiviral and anti-inflammatory activities. Developing efficient extraction and purification workflows for these compounds is essential in natural product research, pharmaceutical development, and quality assurance.

Objectives and Study Overview

The study evaluated a fully supercritical fluid–based workflow to isolate schisandrin A from dried Schisandra berries. Specific aims included:

• Demonstrating supercritical fluid extraction (SFE) to obtain a particulate-free, concentrated crude extract.
• Establishing an analytical supercritical fluid chromatography (SFC) method to identify and quantify schisandrin A.
• Scaling the analytical method to preparative SFC for targeted isolation using mass-directed fraction collection.

Použitá instrumentace

The extraction and purification steps employed:

• SFE 500 System with a 100 mL vessel, operating at 200 bar and 40 °C with a CO₂/isopropanol mixture to generate a 30 mL crude extract.
• ACQUITY UPC 2 System and BEH analytical column for rapid screening, coupled to an ACQUITY QDa mass detector.
• Prep 100q SFC System with a Viridis BEH OBD Prep Column and ACQUITY QDa for mass-triggered collection of target fractions.
• ChromScope, MassLynx/FractionLynx, and Empower 3 software for system control, data acquisition, and processing.

Methodology

Fifty grams of chopped, dried berries underwent dynamic SFE (50 g/min flow, 200 bar, 40 °C) to yield a crude extract requiring no further cleanup. Analytical SFC applied a 1–10% polar modifier gradient (acetonitrile/methanol) over 5 minutes at 1600 psi and 40 °C. The peak at ~1.9 minutes with m/z 417.3 was confirmed as schisandrin A. This method was translated to preparative scale using a 100 mL/min flow, 100 bar backpressure, and 120 µL injections, with fraction collection triggered at m/z 417.

Main Results and Discussion

Analytical chromatograms revealed clear resolution of schisandrin A from co-extractives. Preparative SFC enabled efficient isolation and rapid solvent removal, yielding a fraction whose UV-based purity increased from ~29% in the crude to over 92% after a single run. This demonstrates the high selectivity and throughput of combined SFE–SFC workflows for natural product purification.

Benefits and Practical Applications

• Streamlined workflow: direct transition from SFE to SFC without filtration or evaporation.
• Reduced solvent consumption and faster sample preparation compared to traditional liquid chromatography.
• Scalable, mass-directed purification suitable for research laboratories, pharmaceutical lead generation, and quality control in industrial settings.

Future Trends and Potential Uses

Further developments may include the integration of high-resolution mass spectrometry for improved target identification, automation of preparative SFC processes, and expanded application of supercritical fluid techniques to a broader range of natural products. Such advances will support greener, faster workflows in natural products chemistry and related fields.

Conclusion

The described SFE–SFC approach provides an effective, solvent-efficient strategy for isolating schisandrin A from botanical matrices. With high purity, rapid processing, and minimal post-extraction handling, this method exemplifies modern analytical and preparative chromatography techniques for natural product research.

References

1. Choi Y.H. et al. Optimum SFE Condition for Lignans of Schisandra chinensis Fruits. Chromatographia 48(9/10), 1998.
2. American Herbal Pharmacopoeia and Therapeutic Compendium, Schisandra Berry, Editor Roy Upton, 1999.
3. Zheng S. et al. A Concise Total Synthesis of Deoxyschizandrin and Exploration of Its Antiproliferative Effects. Chem. Eur. J. 2012, 18, 3193–3198.
4. Hudalla C.J. et al. UPC² Strategy for Scaling SFC Methods: Applications for Preparative Chromatography. Waters Application Note, 2014.