水產動物油脂中無機砷之檢驗方法開發   全文下載

Development of the Analytical Method for Inorganic Arsenic in Aquatic Animal Oil

砷以無機砷及有機砷的形態存在，在各種砷化物中，無機砷具有毒性，長期攝入可能會導致癌症。水產動物易因生長環境受污染而累積砷，為暸解國人攝食無機砷之風險，以及配合衛生福利部於108年3月11日預公告修正之「食品中污染物質及毒素衛生標準」，本研究以高效液相層析儀搭配感應耦合電漿質譜儀（HPLC-ICP／MS）開發水產動物油脂中無機砷之檢驗方法。方法前處理以0.28M硝酸溶液於80℃以超音波振盪萃取，利用高效液相層析儀搭配陰離子交換層析管柱，後端再以高靈敏之感應耦合電漿質譜儀進行偵測，可於15分鐘內有效分離無機砷（三價砷與五價砷）及有機砷（雙甲基砷（dimethylarsinic acid, DMA）、單甲基砷（monomethylarsonic acid, MMA）、砷酸甜菜鹼（arsenobetaine, AsB）及砷酸膽鹼（arsenocholine, AsC））等砷化物。以本方法檢測魚油中三價砷及五價砷之定量極限均為0.02mg／kg；添加回收試驗，魚油檢體中三價砷及五價砷之平均回收率分別為89.5－98.0％及91.5－103.3％，變異係數皆小於7％。另以本方法檢測市售16件魚油檢體，結果均未檢出無機砷。本研究方法之前處理流程簡易且耗時短，可應用於魚油中無機砷之例行性檢驗，維護國人健康。

Arsenic can be classified into organic and inorganic compounds. Inorganic arsenic is much more toxic than the organic ones. Aquatic animals may accumulate arsenic due to the contaminated environment. To safeguard the public heath, TFDA actively developed the testing method on the speciation of arsenic in fish oil by high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP/MS). Sample was homogenized and extracted with 0.28 M HNO3 in an ultrasonic bath at 80℃ for 30 min twice. Analytes such as inorganic arsenic (arsenite, arsenate) and organic arsenic (DMA, MMA, AsB, AsC) in the sample solution were separated effectively on an anion exchange column, and detected by ICP-MS in less than 15 min. The calibration curves observed coefficients of determination higher than 0.9995. The limits of quantification for arsenite and arsenate in fish oil were 0.02 mg/kg. The average recoveries of arsenite and arsenate spiked into fish oil were in the range of 89.5-98.0% and 91.5-103.3%, respectively. Surveillance studies contained 16 fish oil samples purchased from markets were conducted. The results showed that inorganic arsenic was not found in all samples. The results also complied with the maximum limits of inorganic arsenic in fish oil listed in ''Sanitation Standards for Contaminants and Toxins in Food'' preannounced by the Ministry of Health and Welfare, Taiwan. The testing method offered fast analysis and simple sample pretreatment, and can be applied into routine testing for the determination of inorganic arsenic in fish oil products for the purpose of public health protection.