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    题名: 以基質固相分散萃取法搭配線上衍生氣相層析串聯式質譜儀檢測環境生物檢體中防曬乳成份含量
    作者: 蔡東穎;Tsai,Dung-Ying
    贡献者: 化學學系
    关键词: 氣相層析;基質固相分散萃取法
    日期: 2013-07-04
    上传时间: 2013-08-22 11:41:10 (UTC+8)
    出版者: 國立中央大學
    摘要: 有機防曬乳成份(organic UV filters)是一種廣泛添加於防曬乳、化妝品以及保養品等各種產品中的化合物,在生產及使用過程中,易由水途徑進入環境中。近年來研究指出脂溶性較高的有機防曬乳成份會累積於魚體中,經由食物鏈累積於人體內,可能會造成內分泌干擾,而危害人體健康,近年來已被歸類為新興汙染物(Emerging contaminants,ECs)的一種。
    本研究是利用基質固相分散萃取法(Matrix solid??? phase dispersion extraction,MSPD)來檢測生物檢體中的有機防曬乳成份,並利用實驗統計設計(statistical experimental design)及變異數分析(analysis of variance,ANOVA)來做最佳化的探討。最佳化後的基質固相分散萃取條件為:以0.5 g生物檢體與1 g矽酸鎂均勻混合,填入含有1 g C18的固相萃取夾中,再用7 ml乙?沖堤出來,並以氮氣吹乾後用內標準品回溶。取10 μL待測物溶液利用大體積樣品導入裝置進行線上(on-line)矽烷化衍生,搭配氣相層析串聯式質譜儀(Gas Chromatography- Tandem mass spectrometry, GC-MS/MS)來偵測,可得偵測極限皆小於0.1 ng/g。在生物檢體中,防曬乳成份的總濃度介於0.5至51.2 ng/g。
    Organic UV filters are a group of chemicals used widely in sunscreen, cosmetic and skin care products to protect skin from damaging UV radiation. After use, organic UV filters are washed off from skin and clothes, and enter the aquatic environment. Recent studies indicate that some lipophilic UV filters can be accumulated in biota and act as endocrine disruptors. Organic UV filters are considered as one kind of the emerging pollutants in the environment.
    In this study, a rapid procedure, Matrix solid-phase dispersion (MSPD), was developed to extract five commonly used organic UV filters: EHS, HMS, BP-3, BP-1 and BP-8, from biota samples. The parameters affecting the MSPD extraction efficiency was systematically investigated by statistical experimental design and analysis of variance. For optimal conditions of MSPD are:0.5 g of fish sample dispersing with 1 g Florisil was packed into the SPE column which contains 1.0 g of octadecyl bonded silica (C18), as the clean-up co-sorbent. The target analytes were then eluted with 7 mL of acetonitrile. The extract was adjusted to 100 L, and on-line derivatized in the GC injection-port with a trimethylsilylated (TMS) reagent. The TMS-derivatives were then identified and quantitated by gas chromatography-tandem mass spectrometry (GCMS/MS). The limits of detection (LODs) were less than 0.1 ng/g. The total concentrations of these organic UV filter residues in biota samples ranged from 0.5 to 51.2 ng/g.
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