Analysis of Diarrheic Shellfish Poison and Lipid Soluble Shellfish Poison

Polymer-based reversed-phase semi-micro column, DE413-2B was used with LC/MS detector to quantify 7 kinds of diarrheic and lipid-soluble shelfish poisons. Generally, mouse has been used for the shellfish poisoning testing, but alternative testing method was required due to animal testing’s long analysis time, low repeatability, and animal right view of points. The LC/MS method is rapid and also determines the compounds that are difficult to be detected using animal testing. DE413-2B can be used in a wide pH range (2-11) with a flexible solvent selection (any portion of 100% water to 100% selected organic solvent).



Sample preparation:
Add 9 mL of 90% (v/v) methanol to shellfish gut
Homogenize for 3~5 minuets
Centrifuge (3,000 rpm, 5 min)
Inject 5 micro-L of superfactant

Sample :
Okadaic acid
Pectenotoxin
Dinophysistoxin
Yessotoxin

Column    : Shodex DE413-2B (2.0mmID*50mm)
Eluent    : (A); 50mM HCOOH + 2mM HCOONH4 aq.
            (B); 50mM HCOOH + 2mM HCOONH4 in (H2O/CH3CN=5/95)
            0 to 5min, 20% (B)
            5 to 12min, 20% (B) to 100% (B)
Flow rate : 0.2mL/min
Detector  : ESI-MS(Negative)

Data provided by Dr.Toshiyuki Suzuki of the Fisheries Research Agency