Determination of Five Lipophilic Marine Toxins in Shellfish by Liquid Chromatography with Tandem Mass Spectrometry
A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method for the determination of five lipophilic marine toxins including Gymnodimine(GYM),Spirolide-1(SPX1),Okadaic acid(OA) Pecenotoxin-2(PTX2) and Azaspiracid-1(AZA1) in shellfish was developed.After being extracted with methanol and water(80 /20,V/V),the extract was cleaned by solid phase extraction of MAX column,then determined by a reversed phase HPLC gradient program coupled with tandem mass spectrometry in selectedreaction-monitoring mode.GYM,SPX1,OA,PTX2,AZA1were analyzed in positive ion mode,while OA in negative ion mode.The calibration curves were linear well between LC peak area of the selected ion-pair and the concentration of five lipophilic marine toxins with the correlation coefficient over 0.99.The average recoveries from spiked scallop muscle at the concentration ranged from 78.6% to 94.4% with relative standard deviation from 6.8% to 14.9%.The limits of detection were 0.10,0.21,2.00,0.32 and 0.04 μg/kg for GYM,SPX1,OA,PTX2 and AZA1 respectively.