Robust and Verified LC-MS/MS Workflow for Screening of Multi-class Veterinary Drug Residues from Various Food Matrices

Significance of the Topic

Veterinary drugs play a critical role in animal health but can accumulate in food products, posing potential risks to consumers. A unified, high-throughput LC-MS/MS workflow enables efficient multi-class screening, ensures compliance with global regulations, and enhances public safety.

Study Objectives and Overview

The aim was to develop and verify a single LC-MS/MS method capable of detecting over 200 veterinary drug residues across diverse chemical classes in nine food matrices. The workflow focuses on high sensitivity, robust performance, and reduced operational cost compared with traditional single-class analyses.

Methodology and Instrumentation

• Target Selection: 210 veterinary drugs chosen based on AOAC, FDA, FSIS, and EU guidelines, representing 28 chemical classes.
• Sample Preparation: Solvent extraction using acidified acetonitrile with EDTA, followed by lipid removal via Agilent Captiva EMR-Lipid cartridges and PPM-48 plates.
• Instrumentation: Agilent 6470 and 6495 triple quadrupole LC-MS/MS systems operating in dynamic MRM mode, coupled with 13-minute Poroshell 120 column chromatography.

Main Results and Discussion

• Sensitivity & Linearity: Over 90% of analytes exhibited LODs ≤ 5 µg/kg; calibration curves were linear (R² ≥ 0.99) up to 100 µg/kg.
• Accuracy & Precision: Recoveries ranged 70–120%; intra-batch signal precision (%RSD) <20%, retention time variability <1%; all targets met inter-batch reproducibility (<32% RSD).
• Robustness: System suitability tests over 400 continuous injections demonstrated stable performance and minimal source contamination.

Benefits and Practical Applications

• High throughput: Cleanup of 48 samples in 30 minutes.
• Rapid analysis: 18-minute injection-to-injection cycle time.
• Regulatory compliance: Suitable for routine QA/QC monitoring of veterinary residues in various animal-derived foods.

Future Trends and Opportunities

• Extension to emerging and non-target veterinary compounds.
• Integration with high-resolution MS for comprehensive screening.
• Automation and real-time data analytics to streamline reporting.

Conclusion

This validated LC-MS/MS workflow offers a robust, sensitive, and efficient approach for multi-class veterinary drug residue screening in food matrices, aligning with global regulatory standards and optimizing laboratory throughput.

Reference

1. AOAC Official Methods, Version 7, 2018.
2. US FDA-CFR Title 21, Part 556, 2019.
3. US FSIS Chemical Contaminants, 2017.
4. EU Commission Regulation 37/2010.
5. Agilent Application Notes 5994-1932EN; 5994-2832EN; 5994-3124EN; 5994-3680EN.