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Extraction of Multiple Mycotoxins From Animal Feed Using ISOLUTE® Myco SPE Columns prior to LC-MS/MS Analysis

Applications | 2013 | BiotageInstrumentation
Sample Preparation, Consumables, LC/MS, LC/MS/MS, LC/QQQ
Industries
Food & Agriculture
Manufacturer
Shimadzu, SCIEX, Biotage

Summary

Importance of the topic

Mycotoxins are fungal metabolites that threaten animal health and feed quality. Reliable detection across diverse feed matrices ensures compliance with regulatory limits and protects animal performance and food safety.

Objectives and study overview

This application note presents a unified SPE protocol using ISOLUTE Myco columns for extracting a panel of major mycotoxin classes from animal feed. The goal is to achieve high recoveries, low limits of quantitation and precision meeting European regulations.

Methodology

Sample preparation includes acidified solvent extraction, centrifugation and dilution. Solid phase extraction uses conditioned ISOLUTE Myco columns with specific wash and elution steps tailored for type B trichothecenes and other mycotoxins. Final extracts are concentrated, reconstituted and filtered before analysis by LC MS MS.

Instrumentation

  • SPE: ISOLUTE Myco 60 mg 3 mL columns
  • UHPLC: Shimadzu Nexera with Kinetex XB C18 50 x 2.1 mm 2.6 micron column
  • MS MS: AB Sciex Triple Quad 5500 with Turbo V ESI source
  • Evaporation: SPE Dry or TurboVap LV
  • Sample handling: Biotage VacMaster manifolds

Main results and discussion

The method delivered linear calibration across each analyte range with correlation coefficients above 0.992. Limits of quantitation met or exceeded EU criteria with values from 1.6 to 900 µg kg 1. Recoveries ranged from 85 to 110 and repeatability RSDs remained below 8 indicating robust performance across soya and horse feed matrices.

Benefits and practical applications

  • Streamlined sample cleanup for multiple mycotoxins using a single SPE product
  • Compatibility with high throughput LC MS MS workflows
  • Compliance with food and feed safety regulations
  • Applicability to diverse feed types and complex matrices

Future trends and possibilities

Advances may include automation of SPE steps, integration with high resolution mass spectrometry for expanded analyte coverage, development of greener solvents and novel sorbent chemistries to improve selectivity and sustainability.

Conclusion

The ISOLUTE Myco SPE protocol demonstrates efficient extraction and cleanup of a broad range of mycotoxins from animal feed. The validated method achieves regulatory performance metrics and supports reliable LC MS MS analysis for feed safety monitoring.

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