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

Materials
related product
CONDITIONS
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
Description
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