技术
LC/MS: suitable
试验参数
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
适用性
application for LC-MS
应用
forensics and toxicology
分析说明
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.
其他说明
mussel tissue homogenate matrix CRM (National Research Council Canada, part no. CRM-ZERO-Mus) extracted with methanol
法律信息
Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
分析物
说明
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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