開發基質固相分散萃取法檢測室內灰塵中的鹵系阻燃劑

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题名:	開發基質固相分散萃取法檢測室內灰塵中的鹵系阻燃劑
作者:	宮敏純;Kung, Min-Chen
贡献者:	化學學系
关键词:	基質固相分散萃取法;鹵系阻燃劑
日期:	2018-06-25
上传时间:	2018-08-31 11:31:31 (UTC+8)
出版者:	國立中央大學
摘要:	鹵系阻燃劑如五溴酚(Pentabromophenol, PeBP)、四氯雙酚A (Tetrachlorobisphenol A, TCBPA)和四溴雙酚A (Tetrabromobisphenol A)廣泛的被添加在電器用品及生活用品中 (如:沙發、窗簾)，在使用與丟棄的過程中阻燃劑可能會釋放到環境，累積在灰塵中。各國的研究也都有發現阻燃劑在灰塵中殘留，我們因此會透過接觸或吸入灰塵，而在體內累積鹵系阻燃劑，對我們產生健康上的影響。　　本研究主要是開發一套簡單且快速檢測這三種鹵系阻燃劑的前處理方法，可以應用在基質複雜的室內灰塵中。利用震盪輔助基質固相分散萃取法 (Vortex-homogenized matrix solid-phase dispersion, VH-MSPD) 進行樣品前處理，搭配超高效液相層析高解析串聯質譜儀(ultra-high performance liquid chromatography quadrupole time-of-flight mass spectrometer, UHPLC-QTOF-MS)進行檢測。　　MSPD的最佳化利用實驗統計設計(Statistical experimental design) 法中的Box-Behnken design (BBD)及變異數分析(Analysis of variance, ANOVA)來做最佳化探討。最佳化的萃取條件為：取0.1 g的灰塵樣品與0.1 g矽酸鎂，放入震盪器中快速混和均勻，再將混和物放入含有0.6 g C18的玻璃管柱中，先使用6 ml的正己烷進行淨化，再加入6 ml的甲醇:乙腈=1:1(v/v)進行沖提並收集，萃取液旋濃乾燥，再以甲醇100 μL進行回溶，取3 μL進樣UHPLC-QTOF-MS進行檢測分析。偵測極限(LOD)為3-15 ng/g；Inter-days及Intra-day的測試所得相對標準偏差(RSDs)皆小於5%，顯示本方法具有良好的穩定性與再現性。在採集的室內灰塵中所測得的鹵化阻燃劑以TBBPA為主，其濃度為70-350 ng/g。 ;Halogenated flame retardants (HFRs) such as pentabromophenol( PeBP ), tetrachlorobisphenol A( TCBPA ), and tetrabromobisphenol A are widely applied in the manufacture of household appliances, daily articles, and furnitures, e.g. sofa and drapes. Due to how common they are, HFRs can be released into the environment during use of previously mentioned items, as shown by recent studies that show HFRs residues in indoor dust. Through dermal contact or inhalation of indoor dust, we may accumulate HFRs in our bodies, which can potentially affect our health. 　　This research developed a simple and rapid method for the determination of three HFRs in complex indoor dusts. This method involved the use of vortex-homogenized matrix solid-phase dispersion (VH-MSPD) coupled with ultra-high performance liquid chromatography quadrupole time-of-flight mass spectrometer (UHPLC-QTOF-MS UHPLC-QTOF-MS). 　　The parameters of the extraction method were optimized by Box-Behnken design and the analysis of variance(ANOVA). The optimal conditions of VH-MSPD were: dispersing 0.1g indoor dust sample with 0.1g Florisil by vigorous shaking to obtain a homogenous mixture. The mixture was transferred to a glass column containing 0.6g of octadecyl bonded silica (C18), which was used as the clean-up co-sorbent along with the addition of 6 mL n-Hexane. The target analytes were then eluted with 6 mL of a mixture of methanol and acetonitrile (1:1,v/v). After rotary evaporation to dryness, the residue was re-dissolved in 100μL of methanol. A fraction of the 3μL final extract was directly injected into UHPLC-QTOF-MS system for detection. 　　The limit of detections (LODs) for these three HFRs in indoor dust samples were determined to be 3-15 ng/g. The relative standard deviations (RSDs) of inter-days and intra-day tests were lower than 5%, and the concentration of TBBPA detected in indoor dust samples ranged from 70-350 ng/g.
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