開發基質固相分散萃取法檢測生物樣品中鹵系阻燃劑

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题名:	開發基質固相分散萃取法檢測生物樣品中鹵系阻燃劑
作者:	陳志明;Chen,Jhih-Ming
贡献者:	化學學系
关键词:	鹵系阻燃劑;基質固相分散萃取法;電子捕捉負離子化學游離法;生物檢體;halogenated flame retardants;matrix solid-phase dispersion;electron capture negative ion;biota sample
日期:	2016-06-20
上传时间:	2016-10-13 12:39:46 (UTC+8)
出版者:	國立中央大學
摘要:	鹵系阻燃劑如：五溴酚 (Pentabromophenol, PeBP)、四溴雙酚A (Tetrabromobisphenol A, TBBPA)、四氯雙酚A (Tetrachlorobisphenol A, TCBPA) 被廣泛添加於民生用品與防火材料中，在生產及使用過程中，容易經由水的途徑而進入環境裡。這類鹵系阻燃劑由於具有較高的親脂性，因此在食物鏈中會累積放大，其殘留濃度也已在水產中被檢測出。本研究主要是發展一套簡單、有效率，可快速檢測這三種鹵系阻燃劑的樣品前處理法，將其應用於不同種類的生物樣品中。利用基質固相分散萃取法 (Matrix solid-phase dispersion, MSPD) 進行樣品前處理，搭配氣相層析質譜儀結合電子捕捉負離子化學游離法 (GC-ECNI-MS) 進行偵測。從生物樣品中萃取目標待測物，並將影響萃取效率之實驗參數，利用實驗統計設計 (Statistical experimental design) Box-Behnken design (BBD) 及變異數分析 (Analysis of variance, ANOVA) 來做最佳化探討。最佳化後的萃取條件為，將0.5 g經由冷凍乾燥的生物樣品與1 g矽酸鎂，放入振盪器中快速均勻混合。將混合物轉移到含有1 g C18的玻璃管柱中，再用12 mL乙腈沖提出來，最後將萃取溶液旋濃乾燥。以內標準品含有衍生試劑回溶進行離線矽烷化衍生，取1 μL待測物溶液利用GC-ECNI-MS進行偵測，可得偵測極限 (LOD) 在0.06-0.15 ng/g間。在inter-days及intra-day的測試中，所得之相對標準偏差 (RSD) 小於7 %，顯示此方法穩定且具有良好的再現性。在生物檢體中，三種鹵系阻燃劑的濃度介於0.3至2.2 ng/g。 ;Halogenated flame retardants, such as pentabromophenol (PeBP), tetrabromobisphenol A (TBBPA), and tetrachlorobisphenol A (TCBPA), are widely used to add in fire protection materials. After production and use, halogenated flame retardants enter the environment easily through the water way. Because of their high lipophilicity, they can be bio-accumulated and bio-magnificated in the food chain. Currently in various aquatic and terrestrial species have detected containing such substances. In this study, a simple and effective method for the rapid analysis of these three halogenated flame retardants in various sea food samples was developed. The method involved the use of vortex-homogenization matrix solid-phase dispersion (VHMSPD) extraction for the sample pretreatment, and determination by gas chromatography-electron capture negative ion mass spectrometry (GC-ECNI-MS). The parameters affecting the extraction efficiency of the target analytes from sea food samples were optimized by Box-Behnken design and analysis of variance. The optimal conditions of VHMSPD involved dispersing of 0.5 g of freeze-dried sea food sample with 1 g of Florisil by a vigorous shaking to obtain a dry homogenous mixture. The mixture was transferred to a glass column containing 1 g of octadecyl bonded silica (C18), as the clean-up co-sorbent. The target analytes were then eluted with 12 mL of acetonitrile. The extract was dried under nitrogen and the residue was redissolved in 50 μL ethyl acetate with internal standard and derivatization regent (BSTFA). Then 1 μL of the derivatized sample was injected to GC-ECNI-MS for analysis. The limits of detection (LODs) were 0.06-0.15 ng/g. Inter-days and intra-day precision (% RSD) for three analytes were less than 7 %. It indicated that the method shows good reproducibility and stability. The total concentrations of these halogenated flame retardants in sea food samples ranged from 0.3-2.2 ng/g.
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