Analysis of Diarrhetic Shellfish Toxines

Importance of Topic

Diarrhetic shellfish toxins are potent marine biotoxins, often causing food poisoning through contaminated bivalve consumption. Rapid and accurate detection is crucial for ensuring seafood safety and protecting public health.

Study Objectives and Overview

The aim of this work is to develop and validate a high-throughput LC–MS method for simultaneous quantification of okadaic acid (OA), dinophysistoxin-1 (DTX1), and dinophysistoxin-2 (DTX2) in scallop samples. The study outlines chromatographic and mass spectrometric conditions to achieve sensitive and reliable measurement of these diarrhetic shellfish toxins.

Methodology

Chromatographic Conditions

• Column: Shim-pack Scepter C18 (100 mm × 2.0 mm I.D., 1.9 µm)
• Mobile phase A: 2 mmol/L ammonium formate in water with 50 mmol/L formic acid
• Mobile phase B: Acetonitrile/water (95/5, v/v) with 2 mmol/L ammonium formate and 50 mmol/L formic acid
• Gradient: 40% B (0–2.5 min) to 100% B (7.5–12.5 min), then back to 40% B (12.51–17.5 min); front cut valve directs eluent to MS during 6–10 min
• Flow rate: 0.2 mL/min; Column temperature: 50 °C; Injection volume: 5 µL

Mass Spectrometric Conditions

• Ionization: Electrospray in negative mode
• Nebulizing gas: 3 L/min; Drying gas: 5 L/min; Heating gas: 15 L/min
• DL temperature: 150 °C; Heat block: 450 °C; Interface temperature: 350 °C
• CID gas: 325 kPa; Probe voltage: –3.0 kV
• MRM transitions: OA 803.30 → 255.10, DTX2 803.30 → 255.10, DTX1 817.30 → 255.10

Main Results and Discussion

The developed method provided clear separation of OA, DTX1, and DTX2 within 10 minutes, with sharp peaks and minimal matrix interference. Sensitivity in MRM mode enabled low detection limits suitable for regulatory compliance.

Practical Benefits and Applications

• High-throughput analysis for routine monitoring of shellfish contamination
• Robust quantification supports quality control in seafood processing facilities
• Efficient sample turnaround aids timely decision-making in public health contexts

Future Trends and Potential Developments

Continuous advancements in UHPLC columns and high-resolution MS may further reduce analysis time and enhance sensitivity. Integration with automated sample preparation and data processing will streamline workflows in regulatory laboratories. Emerging ambient ionization techniques could enable on-site screening of marine toxins.

Conclusion

The UHPLC–MS approach described offers a rapid, sensitive, and reliable solution for quantifying diarrhetic shellfish toxins in scallops. Its application ensures compliance with food safety regulations and supports proactive risk management in the seafood industry.

Reference

Shimadzu Application News C200 (JP, EN)