Accelerated Solvent Extraction (ASE) Sample Preparation Techniques for Food and Animal Feed Samples

Importance of Topic

Accelerated Solvent Extraction (ASE) dramatically streamlines the preparation of solid food and animal feed samples for chemical analysis by reducing solvent consumption, improving reproducibility and recovery, and minimizing manual handling. This approach is essential in food safety, quality control, environmental monitoring, and pharmaceutical residue analysis where high throughput and reliable results are required.

Study Goals and Overview

This technical note presents best practices for using ASE on diverse food and feed matrices. It reviews pretreatment options, in-cell clean-up strategies, solvent selection, and method optimization. A comparative assessment against traditional Mojonnier extraction and a detailed case study of method development for rodent feed illustrate key principles.

Methodology and Instrumentation

• Instrument: Thermo Scientific ASE systems (formerly Dionex ASE 200 and ASE 300).
• Standard ASE Conditions (SAC): 100 °C, 1500 psi (ASE 200), 5 min static, 60 % cell flush, 60–100 s purge, one cycle.
• Pretreatment: Remove moisture by air, oven, freeze, or microwave drying; disperse with diatomaceous earth (ASE Prep DE) or sand; grind to 1–2 mm particle size.
• In-cell clean-up: Add acidic alumina or C18 bonded silica to adsorb lipids and other co-extractables directly in the extraction cell.
• Solvent compatibility: Wide range of organic solvents and aqueous or buffered mixtures; avoid strong mineral acids and caustic solutions to protect system hardware.

Main Results and Discussion

Enhancing sample surface area through grinding and dispersion significantly increases extraction efficiency. Comparison of fat recovery from mozzarella cheese showed ASE at 125 °C matched or exceeded Mojonnier results when samples were finely ground.
Case Study – Rodent Feed:

• Method 1 (75 °C, MeOH, 3 min static): target analyte detected but low recovery.
• Method 2 (150 °C, MeOH, 3 min static): improved recovery but dark, contaminated extract.
• Method 3 (100 °C, MeOH, 5 min static): optimal recovery with clear extract and minimal co-extracted matrix.

Benefits and Practical Applications

• Rapid, reproducible extraction of lipids, pesticides, pharmaceuticals, mycotoxins and other analytes.
• Significant solvent and time savings compared to classical methods.
• Integrated in-cell clean-up reduces downstream purification steps.
• Applicable to a broad spectrum of food, feed, environmental and natural product analyses.

Future Trends and Potential Applications

Emerging developments include integration of ASE with on-line cleanup and hyphenated techniques (ASE–GC/MS, ASE–HPLC), adoption of green solvents, automated method development software, and coupling with high-throughput metabolomics and environmental screening platforms. Miniaturization and robotics will further enhance throughput and reproducibility.

Conclusion

Accelerated Solvent Extraction provides a robust, efficient workflow for preparing food and animal feed samples. By tailoring pretreatment, solvent choice, and extraction parameters, laboratories can achieve high analyte recoveries, clean extracts, and reduced solvent usage while maintaining throughput and reproducibility.

Reference

• Dionex Corporation. Application Note 326: Extraction of Drugs from Animal Feeds Using Accelerated Solvent Extraction (ASE).
• Dionex Corporation. Application Note 349: Rapid Determination of Organochlorine Pesticides in Animal Feed Using ASE.
• Dionex Corporation. Application Note 353: Rapid Determination of Sulfonamide Residues in Animal Tissue and Infant Food.
• Dionex Corporation. Application Note 322: Selective Extraction of PCBs from Fish Tissue Using ASE.
• Dionex Corporation. Application Note 321: Determination of Unbound Fat in Various Food Matrices Using ASE.
• Dionex Corporation. Application Note 329: Determination of Total Fat in Powdered Infant Formula Using ASE.
• Dionex Corporation. Application Note 332: Accelerated Solvent Extraction of Pesticide Residues in Food Products.
• Dionex Corporation. Application Note 334: Rapid Determination of Fat in Meat Using ASE.
• Dionex Corporation. Application Note 335: Extraction of Active Ingredients from Natural Products.
• Dionex Corporation. Application Note 340: Determination of Fat in Dried Milk Products Using ASE.
• Dionex Corporation. Application Note 342: Determination of PCBs in Large Volume Fish Tissue Samples Using ASE.
• Dionex Corporation. Application Note 343: Determination of Pesticides in Large Volume Food Samples Using ASE.
• Dionex Corporation. Application Note 344: Extraction of Fat from Chocolate Using ASE.
• Dionex Corporation. Application Note 345: Extraction of Fat from Dairy Products Using ASE.
• Dionex Corporation. Application Note 350: Extraction of Zearalenone from Wheat and Corn by ASE.
• Dionex Corporation. Application Note 409: Fast Determination of Acrylamide in Food Using ASE/ICUV or ASE/ICMS.
• Gentili A.; Perret D.; Marchese S.; Sergi M.; Olmi C.; Curini R. Accelerated Solvent Extraction and Confirmatory Analysis of Sulfonamide Residues in Raw Meat and Infant Foods by LC–ESI–MS/MS. J. Agric. Food Chem. 2004, 52, 4614–4624.