Accelerated Solvent Extraction Techniques for In-Line Selective Removal of Interferences

Significance of the Topic

Accelerated Solvent Extraction ASE with in-cell adsorbents integrates extraction and clean-up in one step reducing solvent consumption and improving sample throughput. This approach addresses co-extraction of interferences such as lipids sulfur compounds and pigments from environmental food biological and industrial matrices ensuring reliable downstream analysis by GC HPLC LC MS and other techniques.

Objectives and Study Overview

This note reviews seven ASE based workflows aiming to selectively remove interferences or fractionate target analytes during extraction. These include selective extraction of nonpolar compounds polar contaminants lipid fractionation and analyte cleanup across diverse matrices.

Methodology and Instrumentation

Each method employs Thermo Scientific Dionex ASE systems combined with in-cell adsorbents tailored to the analyte and matrix.

• Nonpolar cleanup adsorbents: alumina acid impregnated silica gel C18 Florisil activated carbon
• Polar analytes: OnGuard II ion exchange resins strong base chelating cartridges
• Lipid fractionation: sequential solvent program hexane acetone chloroform methanol
• Sample preparation aids: glass fiber and cellulose filters sodium sulfate Ottawa sand
• Instrumentation: Dionex ASE 200 accelerated solvent extractor HPLC GC MS LC MS MS

Main Results and Discussion

• Alumina retains nonpolar lipids during PCB extraction from fish tissues and meal enabling direct GC analysis.
• Acid impregnated silica gel eliminates lipids in PCB extraction from meal improving selectivity.
• OnGuard ion exchange resins enable direct extraction of perchlorate from vegetation in water eliminating post cleanup.
• C18 resin coupled with cooling and centrifugation effectively removes nonpolar lipids for sulfonamide and corticosteroid residue analysis by LC MS MS.
• Florisil in-cell cleanup reduces visible coextractives for acrylamide analysis in coffee and cocoa.
• Sequential solvent extraction fractionates neutral lipids and phospholipids in one run enabling targeted lipid class analysis.

Benefits and Practical Applications

• Combines extraction and clean up reducing steps solvent usage and labor.
• Enhances analyte purity lowers instrument maintenance.
• Adaptable to environmental food feed clinical and industrial QC workflows.
• Compatible with regulatory methods including EPA protocols.

Future Trends and Applications

Integration of novel sorbent materials and miniaturized ASE platforms will expand target analyte scope. Coupling ASE with online LC MS and high resolution mass spectrometry promises fully automated sample to result workflows. Green solvent development and programmable fractionation will enhance sustainability and selectivity for emerging contaminants and complex lipidomics.

Conclusion

In-cell cleanup using ASE enables streamlined selective extraction across various matrices. The approach reduces solvent usage time and cleanup steps while delivering high quality extracts ready for direct instrumental analysis. Continued innovation in adsorbent chemistry and automation will broaden applicability in analytical chemistry.

References

1. Nording M Sporring S Wiberg K Bjorklund E Haglund P Monitoring Dioxins in Food and Feedstuffs Using Accelerated Solvent Extraction with a Novel Integrated Carbon Fractionation Cell in Combination with Bioassay Anal Bioanal Chem 2005 381 1472-1475
2. US EPA Method 3660B Sulfur Cleanup US Environmental Protection Agency Cincinnati OH 1996
3. Dionex Determination of Perchlorate in Vegetation Samples Using Accelerated Solvent Extraction and Ion Chromatography Application Note 356 LPN 1807 Thermo Fisher Scientific 2006
4. Dionex Rapid Determination of Sulfonamide Residues in Animal Tissue and Infant Food Using Accelerated Solvent Extraction Application Note 353 LPN 1708 Thermo Fisher Scientific 2005
5. Bjorklund E Muller A von Holst C Comparison of Fat Retainers in Accelerated Solvent Extraction for the Selective Extraction of PCBs from Fat-Containing Samples Anal Chem 2001 73 4050-4053
6. Sporring S Bjorklund E Selective Pressurized Liquid Extraction of Polychlorinated Biphenyls from Fat-Containing Food and Feed Samples J Chromatogr A 2004 1040 155-161
7. Ezell J Richter B Francis E Selective Extraction of PCBs from Fish Tissue Using Accelerated Solvent Extraction American Environmental Laboratory 1996 12 12-13
8. Dionex Selective Extraction of PCBs from Fish Tissue Using Accelerated Solvent Extraction Application Note 322 LPN 0764 Thermo Fisher Scientific 1996
9. Dionex Determination of PCBs in Large-Volume Fish Tissue Samples Using Accelerated Solvent Extraction Application Note 342 LPN 1204 Thermo Fisher Scientific 2000
10. Gomez Ariza JL Bujalance M Giraldez I Velasco A Morales E Determination of Polychlorinated Biphenyls in Biota Samples Using Simultaneous Pressurized Liquid Extraction and Purification J Chromatogr A 2002 946 209-219
11. US EPA Method 3620C Florosil Cleanup US Environmental Protection Agency Cincinnati OH 2000
12. Gomez Ariza JL Garcia Barrera T Lorenzo F Gonzales A Optimisation of a Pressurised Liquid Extraction Method for Haloanisoles in Cork Stoppers Anal Chim Acta 2005 540 17-24
13. Draisci R Marchiafava C Palleschi L Cammarata P Cavalli S Accelerated Solvent Extraction and Liquid Chromatography Tandem Mass Spectrometry Quantitation of Corticosteriod Residues in Bovine Liver J Chromatogr B Anal Technol Biomed Life Sci 2001 753 217-223
14. Gentili A Perret D Marchese S Sergi M Olmi C Curini R Accelerated Solvent Extraction of Confirmatory Analysis of Sulfonamide Residues in Raw Meat and Infant Foods by LC Electrospray Tandem Mass Spectrometry J Agric Food Chem 2004 52 4614-4624
15. Dionex Extraction and Clean Up of Acrylamide in Complex Matrices Using ASE Followed by LC MS MS Application Note 358 LPN 1871 Thermo Fisher Scientific 2006
16. Poerschmann J Carlson R New Fractionation Scheme for Lipid Classes Based on In-Cell Fractionation Using Sequential Pressurized Liquid Extraction J Chromatogr A 2006 1127 18-25
17. Poerschmann J Trommler U Biedermann W Truyen U Lucker E Sequential Pressurized Liquid Extraction to Determine Brain Originating Fatty Acids in Meat Products as Markers in BSE Risk Assessment Studies J Chromatogr A 2006 1127 26-33