マガキ中の下痢性貝毒分析における前処理法の簡易化とその妥当性評価

抄録

A method for analysis of okadaic acid (OA), dinophysistoxin-1 (DTX1) and dinophysistoxin-2 (DTX2) using deproteination cartridge filter was developed. This is a simple method because it does not require complicated operations such as conditioning and washing of the column. The shellfish poisons in oyster were extracted with methanol and methanol/water (9:1), and were hydrolyzed with 2.5 mol/L sodium hydroxide solution. The crude extracts were defatted by liquid- liquid partition using n-hexane, and were passed through a deproteination cartridge filter. Measurement was performed by liquid chromatography tandem mass spectrometry. As a result of the validation study using the matrix calibration curve method, the trueness, repeatability and withinlaboratory reproducibility were 92-98, 1.0-3.0 and 2.0-4.0%, respectively, and met the target values of notification of Ministry of Health, Labour and Welfare of Japan.