Extraction of Acrylamide from Cooked Foodstuffs Using ISOLUTE® Multimode Columns

Significance of the Topic

Acrylamide is a small, water soluble compound formed in high temperature cooking processes and is classified as a potential carcinogen. Reliable detection of trace levels of acrylamide in foodstuffs is essential for consumer safety and regulatory compliance. The development of an efficient clean-up and quantification strategy addresses challenges presented by complex food matrices.

Study Objectives and Overview

The focus of this work is to outline a sample preparation and LC-MS/MS method for the extraction and quantification of acrylamide from cooked foods. The study utilizes ISOLUTE Multimode solid phase extraction columns that combine hydrophobic, cation and anion exchange interactions to remove matrix interferences while allowing acrylamide to pass through for analysis.

Methodology

• Sample Preparation
  • Homogenize 2-4 g of cooked sample with 40 mL water
  • Add 800 µL of deuterated acrylamide internal standard (2.0 µg/mL)
  • Homogenize at 9500 rpm for 2 minutes
  • Centrifuge at 3600 g for 10 minutes and collect the supernatant
• SPE Clean-Up with ISOLUTE Multimode 300 mg/3 mL
  • Condition column with 1 mL acetonitrile
  • Equilibrate with two 2 mL water rinses
  • Load 3 mL of sample extract
  • Discard initial 1 mL of eluent; collect the remainder containing acrylamide
  • Filter through 0.22 µm syringe filter; further clarify using 16 800 g spin filter
• Optional Preconcentration
  • Use ISOLUTE ENV+ SPE if additional concentration is required

Instrumentation Used

• Solid Phase Extraction: ISOLUTE Multimode SPE columns (300 mg/3 mL)
• Organic solvents: HPLC-grade acetonitrile and Milli-Q water
• Internal standard: Deuterated acrylamide at 2.0 µg/mL
• Analytical system: Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)
• Filtration: 0.22 µm syringe filters and centrifuge spin filters
• Centrifuges capable of 3600 g and 16 800 g

Main Results and Discussion

The multimode SPE approach effectively retains hydrophobic and ionic interferences while allowing acrylamide to remain unretained and subsequently collected. The combined washing and filtering steps yield a clean sample suitable for LC-MS/MS analysis. This method provides high recovery and reproducibility across various food matrices such as potato crisps and other cooked products. Additional freezing and centrifugation steps may be used for high-fat or particulate-rich samples.

Benefits and Practical Applications

• Enhanced selectivity through multimodal retention mechanisms
• Reduced matrix effects in LC-MS/MS quantification
• Scalable and adaptable to different food matrices
• Compatible with high throughput workflows in QA/QC and research laboratories

Future Trends and Applications

• Integration with high-resolution mass spectrometry for improved specificity
• Automation of SPE workflows for increased throughput
• Miniaturization of sample preparation techniques to reduce solvent consumption
• Expansion to monitor other processing-related contaminants in food

Conclusion

The described method offers a robust and reliable workflow for extracting and quantifying acrylamide from cooked foods. By employing an ISOLUTE Multimode SPE clean-up combined with LC-MS/MS detection, laboratories can achieve sensitive, accurate, and reproducible results essential for food safety monitoring.

Reference

• Rosen J et al Analysis of acrylamide in cooked foods by liquid chromatography tandem mass spectrometry Analyst 2002 127 880-882