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Merck
CN

G1006630

LC/MS/MS Analysis of Marine Toxins in Shellfish According to EU Regulations on Ascentis® Express C18

application for LC-MS

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technique(s)

LC/MS: suitable

test parameters

column: Ascentis Express C18, 10 cm x 2.1 mm I.D., 2 μm particles (50813-U)
mobile phase: [A] 2mM ammonium acetate with 0.1% formic acid in acetonitrile:water (5:95), [B] 2 mM ammonium acetate with 0.1% formic acid in acetonitrile:water (95:5)
gradient: 20% to 80% B in 4 min, to 95% B in 1 min, held at 95% B for 1 min, to 20% B in 0.5 min, held at 20% B for 1.5 min
flow rate: 0.6 mL/min
pressure: 5801 psi (400 bar)
column temp.: 40 °C
detector: MS/MS ESI(+) and ESI(-), MRM (see Figure for transitions)
injection: 10 μL

suitability

application for LC-MS

application(s)

forensics and toxicology

Analysis Note

Biotoxins in shellfish have recently come under increased scrutiny. The European Union (EU) has issued regulation changes requiring all shellfish commodities to be tested for levels of these toxins. Shown here is a rapid and reproducible method for the extraction and analysis of lipophilic marine toxins from shellfish. Separation was achieved in less than seven minutes on an Ascentis® Express C18 column. Recoveries ranged from 80-120% using matrix-matched calibration standards. Certified reference materials provided reliable quantification.

Other Notes

mussel tissue homogenate matrix CRM (National Research Council Canada, part no. CRM-ZERO-Mus) extracted with methanol

Legal Information

Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany

Analyte

Description
    Gymnodimine solution, 9.9 μM in methanol, certified reference material
    Azaspiracid-1 solution, 1.47 μM in methanol, certified reference material
    Dinophysistoxin-1 solution, 18.5 μM in methanol, certified reference material

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