Abstract
A liquid chromatography-tandem mass Spectrometric method for the determination of diarrhetic shellfish poisoning including okadaic acid(OA) and dinophysistoxins-1(DTX-1) in mussel. After being extracted using methanol and water(80:20,V/V),The solution was defatted with n-hexane and extracted in chloroform. After being concentrated ,the residue was dissolved with n-hexane and acetone(20:80,V/V).Then the solution was cleaned-up by solid phase extraction(SPE) on an Si cartridge.The analytes were eluted with methanol - acetone(40:60,V/V). The quantitative and confirmatory determination of OA and DTX-1 were performed by MRM mode. OA and DTX-1 were determined in the negative ion mode. The calibration curves were linear. The method was accurate and reproducible, being successfully applied to the monitoring of OA and DTX-1.The recoveries of standard addition levels were 92.5%-96.7%. The relative standard deviations were all below 6.67%. The limit of quantitation (LOQ) for this method as defined by ten times signal to noise was 20μg/kg.
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