ANALYSIS OF SULFONAMIDES AND QUINOLONES IN SHRIMP USING THE AGILENT 6460 TRIPLE QUADRUPOLE LC/MS

Significance of the topic

The monitoring of sulfonamide and quinolone residues in shrimp is critical for food safety and public health. Veterinary use of these antibiotics can lead to residual levels in seafood that foster antibiotic resistance. Regulatory authorities enforce maximum residue limits (MRLs) to protect consumers and ensure compliance in food production.

Objectives and study overview

This application demonstrates a rapid, sensitive method to quantify twenty-five sulfonamide and quinolone antibiotics in shrimp using QuEChERS extraction coupled to Agilent 6460 Triple Quadrupole LC/MS. The goal is to achieve reliable, matrix-matched calibration and high recovery for routine monitoring.

Methodology and instrument used

Sample preparation applied the QuEChERS protocol:

• Homogenise 2 g shrimp and spike with standards at defined levels.
• Extract with acidified acetonitrile and QuEChERS salts, vortex and centrifuge.
• Clean up with dispersive-SPE, evaporate and reconstitute in methanol/water (50:50).

Chromatography and mass spectrometry:

• UHPLC: Agilent 1290 Infinity with RRHD Zorbax Eclipse Plus C18 column (3.0×100 mm, 1.8 μm), 5 mM ammonium formate/0.1% formic acid (A) and 0.1% formic acid in acetonitrile (B), gradient from 10% to 95% B in 11 min, flow 0.5 mL/min, 30 °C.
• MS/MS: Agilent 6460 Triple Quadrupole with JetStream ESI in positive mode, gas temp 300 °C, sheath gas 400 °C, capillary 2 500 V, dynamic MRM acquisition.

Main results and discussion

Matrix-matched calibrations from 2.5 to 100 ppb delivered linear responses (R² > 0.995) for all targets. Spiking recovery tests at 10, 15 and 25 ng/g showed mean recoveries over 98% across the analyte panel. The method provided low limits of quantitation, minimal matrix effects and high reproducibility, suitable for regulatory compliance.

Benefits and practical applications

This workflow offers:

• High throughput screening of multiple antibiotic residues in seafood.
• Robust quantitation with matrix compensation.
• Compatibility with routine QA/QC labs for compliance with MRL regulations.

Future trends and potential applications

Advances in high-resolution mass spectrometry and automated sample preparation are expected to further improve sensitivity and reduce analysis time. Integration with laboratory information management systems (LIMS) and data-driven quality control will enhance traceability. Expanded multi-residue methods may include additional veterinary drugs and emerging contaminants.

Conclusion

The developed QuEChERS-LC/MS/MS method on the Agilent 6460 provides a rapid, sensitive, and robust solution for monitoring sulfonamides and quinolones in shrimp. It meets regulatory requirements for residue analysis and supports food safety programs by delivering reliable quantitation and high recovery.