建立水產品潛在六溴環十二烷新興污染物質分析與含量調查之研究

六溴環十二烷(Hexabromocyclododecane, HBCD)為溴化阻燃劑，常應於漁業、水產養殖用具如保麗龍浮具、漁網、釣魚線等塑膠製品。HBCD易影響生物體之內分泌系統、具有神經毒性潛能，HBCD於環境中不易分解且可能會透過食物鏈進入到人體造成食用危害風險。目前台灣尚未針對水產品之HBCD含量之相關與調查研究，因此，本研究利用分散固相萃取結合液相層析串聯式質譜儀發展一套對於水產品中HBCD之檢測分析技術並應用於真實樣品調查與評估。樣品前處理最佳化方法結果顯示，精秤5 g均質樣品加入10 mL純水振盪1分鐘後，加入10 mL乙腈振盪萃取5分鐘，再分別加入4 g 無水硫酸鎂、3 g 氯化鈉，振盪1分鐘，並每分鐘3309xg離心15分鐘，吸取上清液2 mL至裝有C18吸附劑 200 mg、一級二級胺吸附劑20 mg及無水硫酸鎂300 mg之15 mL離心瓶中振盪1分鐘並每分鐘3309xg離心15分鐘，吸取淨化液1 mL吹氮濃縮至乾，並以1 mL甲醇回溶過濾以LC-MS/MS進行分析。其結果顯示回收率平均值為110%，相對標準偏差為3.10%，檢量線R2>0.9978，最低偵測極限為0.55 μg kg-1，定量極限為1.80 μg kg-1。本研究方法成功應用於水產品中HBCD之分析，調查樣品(大型魚類及牡蠣) 之HBCD均低於偵測極限，本研究結果有助於了解台灣目前有關HBCD在水產品上之污染程度提升國內有關食品潛在污染之研究能力，並監測水產品中HBCD之含量來達到食品安全管理之效益。

關鍵字

六溴環十二烷；分散固相萃取；液相層析質譜儀；水產品；食品安全

並列摘要

Hexabromocyclododecane (HBCD) is a brominated flame retardant and is used in fishery and aquaculture equipment such as Styrofoam buoys, fishing nets, fishing lines and other plastic products. According to toxicity testing in animals, the HBCD may disturb the thyroid and endocrine systems and is potentially neurotoxic. HBCD is not easily decomposed in the environment. Through the food chain, the HBCD can enter the human body. Currently, no investigation has been conducted in Taiwan into the HBCD content in aquatic products. Therefore, the research objective was to develop a dispersive solid phase extraction technique that can be used in conjunction with liquid chromatography tandem mass spectrometry. This method is then applied to monitor the HBCD content in edible aquatic products commonly found in Taiwan. The results of the optimized method of sample pretreatment showed that the 5 g sample was weighed mixed with 10 mL H2O. Subsequently, 10mL acetonitrile was added to shake for 1 minutes. In the next step, 4 g anhydrous magnesium sulfate and 3 g sodium chloride were added to shake for 1 minute and centrifuged for 15 min at 3309xg. In the next step, 2 mL crude extract from the upper, organic layer was transferred to a new 15-mL PP tube containing 200 mg of C18 adsorbent, 20 mg of primary and secondary amine adsorbent, and 300 mg of anhydrous magnesium sulfate. The tube was shaken for 1 min and centrifuged for 15 min at 3309xg. The supernatant (1 mL) were concentrated to complete dryness with nitrogen blowing and then dissolved in 1mL of methanol for LC-MS/MS analysis. This method was validated and exhibited favorable performance as well as acceptable accuracy (110%), precision (standard deviations <3.10%), R2>0.9978, sensitivity (limits of detection was 0.55 μg kg-1, limits of quantification was 1.80 μg kg-1).This methodology has been successfully applied in analyzing various aquatic products from local markets. The results of our study are helpful to understand the current pollution of HBCD in fishery products in Taiwan. This study is expected to provide crucial insights into food safety management as well as the formulation of food management strategies and food policies.