Quantitative Screening of Multiresidue Veterinary Drugs in Seafood Using the Agilent 6470 Triple Quadrupole LC/MS

Significance of the Topic

Multiresidue analysis of veterinary drugs in seafood is critical for ensuring food safety, meeting global maximum residue limit regulations, and protecting consumer health. Seafood matrices like shrimp and salmon present complex lipid content that challenges reliable detection of low-level drug residues.

Objectives and Overview

This work evaluates the Agilent Comprehensive Veterinary Drug dynamic MRM solution for quantitative screening of 210 veterinary drugs in shrimp and salmon. The focus is on method sensitivity, linearity, precision, accuracy, recovery, matrix effects, and applicability for routine multiresidue monitoring.

Methodology

Sample preparation employs solvent extraction followed by lipid removal using Captiva EMR-Lipid cartridges under positive pressure. Matrix-matched calibration covers 0.1 to 100 μg/kg levels in final extracts. Chromatographic separation is achieved with a Poroshell 120 EC-C18 column and a 13-minute gradient. Detection uses an Agilent 6470 triple quadrupole LC/MS in dynamic MRM mode with fast polarity switching. Data processing relies on matrix-matched calibration curves and rigorous criteria for signal-to-noise, accuracy, and precision.

Used Instrumentation

• Agilent 1290 Infinity II LC System (pump, multisampler, column thermostat)
• Agilent InfinityLab Poroshell 120 EC-C18 column
• Agilent 6470 Triple Quadrupole LC/MS with Jet Stream source
• Agilent positive pressure manifold (PPM-48) and Captiva EMR-Lipid cartridges

Main Results and Discussion

Limits of detection reached as low as 0.1 μg/kg for many targets, with LOQ typically at five times the noise threshold. All 210 analytes showed linear calibration (R2 > 0.99) over the tested range. Response precision (RSD) was below 14% and retention time variability under 0.4%. Recovery for over 93% of compounds fell within 60–120%, with intrabatch RSD ≤ 20%. Matrix effects were minor for most analytes, with suppression below 25%. Method transfer to the 1260 Infinity II Prime LC system yielded comparable chromatographic performance. Verification on an Agilent 6495C LC/TQ confirmed enhanced sensitivity.

Benefits and Practical Applications

This workflow offers a streamlined, robust approach for high-throughput screening of multiclass veterinary drugs in lipid-rich seafood. It fulfills regulatory requirements, minimizes matrix interferences, and supports routine quality control in food testing laboratories.

Future Trends and Possibilities for Application

The approach may be extended to additional seafood species, integrated with high-resolution mass spectrometry for non-targeted screening, and combined with automation and artificial intelligence for rapid data evaluation. Emerging sample-cleanup media and microflow LC could further enhance sensitivity and throughput.

Conclusion

The Agilent Comprehensive Veterinary Drug dMRM solution delivers sensitive, accurate, and reproducible screening of over 200 veterinary drugs in shrimp and salmon matrices. It meets stringent regulatory standards and adapts to diverse LC/MS platforms, making it well suited for routine monitoring of seafood safety.

References

1. An End-To-End Workflow for Quantitative Screening of Multiclass, Multiresidue Veterinary Drugs in Meat Using the Agilent 6470 Triple Quadrupole LC/MS, Agilent Technologies application note, publication 5994-1932EN, 2020
2. AOAC Guidelines on Screening and Identification Method for Regulated Veterinary Drug Residues in Food, Version 7, June 20, 2018
3. Title 21 Code of Federal Regulations, Part 556 Tolerance of Residues in New Animal Drugs in Food, April 1, 2019
4. FSIS Chemical Contaminants of Public Health Concern, USDA Food Safety and Inspection Service, 2017
5. Commission Regulation (EU) No 37/2010 on Pharmacologically Active Substances and Classification Regarding Maximum Residue Limits, Official Journal of the European Union
6. Comprehensive Veterinary Drug dMRM Solution Workflow Guide (G5368AA), Agilent Technologies