A Fast Sample Preparation Workflow for Veterinary Drugs Analysis in Salmon - Using Agilent Captiva EMR—Lipid and LC/MS/MS

Significance of the Topic

Monitoring veterinary drug residues in seafood such as salmon is essential for food safety and public health, helping regulators ensure compliance with maximum residue limits in major markets worldwide.

Study Objectives and Overview

The study aimed to develop a streamlined, one-step sample preparation and targeted LC/MS/MS method capable of quantifying 53 veterinary drugs across seven chemical classes in salmon matrices. By integrating extraction and cleanup, the workflow seeks to improve efficiency and reproducibility.

Methodology and Instrumentation

Sample preparation involved:

• Weighing 2 g of homogenized salmon and spiking with analyte standards and isotopically labeled surrogates.
• Extracting with 9 mL of acetonitrile/water/formic acid (80/5/5) using a Geno/Grinder, followed by centrifugation.
• Cleaning the extract via gravity-driven pass-through on a 3 mL Agilent Captiva EMR—Lipid cartridge.

The cleaned eluate was directly injected (2 µL) into an Agilent 1290 Infinity LC system equipped with an InfinityLab Poroshell 120 EC-C18 column, coupled to an Agilent 6495B triple quadrupole MS with Jet Stream electrospray ionization. MRM transitions were optimized for each analyte according to retention times and collision energies.

Key Results and Discussion

The method exhibited strong linearity (R² 0.993–0.999) over 0.1–100 ng/g, with matrix-matched calibration. Accuracy and precision were evaluated at low, mid, and high QC levels, yielding recoveries between 70 and 120% for 96% of the 53 drugs and relative standard deviations under 20% in most cases. The one-step extraction with 5% formic acid provided superior recoveries compared to other solvent compositions.

Benefits and Practical Applications

This workflow offers:

• Rapid turnaround with minimal hands-on time.
• Robust cleanup of lipophilic matrix interferences.
• High sensitivity and reproducibility suitable for routine regulatory and quality control analysis.

Future Trends and Potential Applications

Further developments may include adapting the protocol to diverse seafood and animal tissue matrices, integrating automated SPE platforms, and expanding to high-resolution accurate mass detection for untargeted screening of emerging contaminants.

Conclusion

A fast, simple, and reliable sample preparation combined with LC/MS/MS analysis on Agilent platforms enables comprehensive quantification of a broad spectrum of veterinary drug residues in salmon, supporting regulatory monitoring and food safety programs.

Instrumentation

• Agilent 1290 Infinity LC
• Agilent 6495B triple quadrupole LC/MS with Jet Stream ESI
• Agilent InfinityLab Poroshell 120 EC-C18, 3.0×100 mm, 2.7 µm column
• SPEX Geno/Grinder for sample homogenization
• Agilent Captiva EMR—Lipid cartridges (3 mL, 300 mg)

Reference

1. Love DC et al. Veterinary drug residues in seafood inspected by the European Union, United States, Canada, and Japan from 2000 to 2009. Environ Sci Technol. 2011;45:7232–7240.