| 中文摘要 |
氨代螺旋酸（azaspiracid, AZA）為脂溶性的海洋毒素，主要是由微型甲藻所產生的代謝產物，雙殼貝類經由濾食，將氨代螺旋酸累積於貝肉組織中，人類誤食經氨代螺旋酸污染之貝類後，造成噁心，嘔吐，腹瀉及胃痙攣等中毒症狀，稱為氨代螺旋酸貝毒（azaspiracid poisoning, AZP）。有鑑於國際間發現貝類中氨代螺旋酸貝毒之案例，且本署預告訂定之「食品中汙染物質及毒素衛生標準草案」訂有其限量，故擬建立該檢驗方法。本研究取均質後之雙殼貝檢體以甲醇萃取氨代螺旋酸後，利用液相層析串聯質譜儀（liquid chromatograph／tandem mass spectrometer, LC／MS／MS）採多重反應偵測（multiple reaction monitoring, MRM）模式進行分析。選用竹蛤空白檢體進行添加回收試驗，添加濃度為2及10ng／g，氨代螺旋酸AZA-1、AZA-2及AZA-3之五重複平均回收率介於72.6－108.6％之間，變異係數（CV％）皆小於15％，本檢驗方法之定量極限為0.002mg／kg。以建立之方法分析貝類標準參考物質CRM-AZA-Mus，AZA-1、AZA-2及AZA-3檢測值分別為1.42、0.314及0.203mg／kg與標示值1.16、0.273及0.211mg／kg略為接近，顯示本方法之準確性佳。另抽驗市售13件雙殼貝類檢體，檢驗結果皆未檢出。
Azaspiracids (AZAs) are lipophilic polyether marine toxins that accumulate in various shellfish species in the tissue of bivalves through filter-feeding. Humans ate poisonous shellfish containing AZAs may cause nausea, vomiting, diarrhea, and stomach cramps, known as azaspiracids poisoning (AZP). In view of the incidents of AZP were happened internationally, this study aimed on the establishment of the analytical method for azaspiracids in foods. Liquid chromatograph/ tandem mass spectrometer (LC/MS/MS) with the multiple reaction monitoring mode (MRM) was applied. Bivalves samples were homogenized, extracted with methanol and analyzed by LC/MS/MS. Recovery studies were performed by spiking of 2 and 10 ng/g standards (AZA1-3) into blank calm samples. The average recoveries were between 72.6 and 108.6% and the coefficients of variation were between 2.8 and 1.8%. The limit of quantitation was 0.002 mg/kg. The established method was validated by testing of certified reference material (CRM-AZA-Mus). The detected values of AZA-1, AZA-2, and AZA-3 in CRM was 1.42, 0.314, and 0.203 mg/kg, respectively, which were closed to the certified value of 1.16, 0.273, and 0.211 mg/kg. Thirteen commercial samples of bivalves were surveyed. The results showed AZA-1, AZA-2, and AZA-3 were not found in all samples. |
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