以基質固相分散萃取法快速檢測生物樣品中之氯化耐燃劑; Rapid determination of Dechlorane Plus and Dechloranes in biota samples by matrix solid-phase dispersion and gas chromatography – electron-capture negative ion mass spectrometry

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题名:	以基質固相分散萃取法快速檢測生物樣品中之氯化耐燃劑;Rapid determination of Dechlorane Plus and Dechloranes in biota samples by matrix solid-phase dispersion and gas chromatography – electron-capture negative ion mass spectrometry
作者:	陳建良;Chen,Chien-Liang
贡献者:	化學學系
关键词:	氯化耐燃劑;基質固相分散萃取法;氣相層析儀;電子捕捉負離子化學游離法;質譜儀;生物樣品;Dechlorane Plus;matrix solid-phase dispersion;gas chromatography;electron-capture negative ion;mass spectrometry;biota samples
日期:	2013-07-02
上传时间:	2013-08-22 11:41:19 (UTC+8)
出版者:	國立中央大學
摘要:	氯化耐燃劑(如Dechlorane Plus, Dechlorane 602, Dechlorane 603 及 Dechlorane 604)，已經被使用了很長一段時間，主要是為了取代具有急毒性的滅蟻靈(Mirex)。當開始使用時並沒有注意到排放到環境中的Dechlorane Plus和其相關化合物具有生物累積性和生物放大的特性。直到2006年，才於文獻中第一次被報導出，這類氯化耐燃劑具有持久性和非常高的親脂性(log KOW>9)，因此在食物鏈中累積，其殘留濃度也常在水產中被檢測到。本篇研究主要是發展一套簡單、有效率，可快速檢測這五種氯化耐燃劑的樣品前處理方法，以便應用在不同種類生物樣品中進行萃取。使用基質固相分散萃取法(Matrix solid-phase dispersion, MSPD)來做樣品前處理，並利用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，並把會影響萃取效率的實驗參數，利用實驗設計法中的Box-Behnken design來進行最佳化。最佳化的實驗條件為，把1 g經由冷凍乾燥的生物樣品和2 g的SiO2，放入振盪器中快速均勻混合。把混合物轉移到含有1 g矽酸鎂的玻璃管柱中，利用矽酸鎂作為共吸附劑和淨化的作用，並用20 mL的正己烷進行沖提。再將萃取液旋濃至1 mL並定溶。回溶後取1 μL萃取液利用GC-ECNI-MS進行偵測，偵測極限可低至0.6 - 2 pg/g。實驗結果初步顯示，在各種水生樣品中都有檢測到微量的四種氯化耐燃劑。 Dechlorane Plus, Dechlorane 602, Dechlorane 603 and Dechlorane 604 are chlorinated flame retardants that have been widely used as the substitution for mirex, but they have not been noticed as environmental contaminants until 2006. Regardless of their large molecular size and very high lipophilicity (log KOW > 9), Dechlorane Plus and related compounds have been detected in various aquatic and terrestrial species, supporting their bioaccumulation and biomagnification. A simple and effective method for the rapid analysis of five chlorinated flame retardants in various biota sample is described. The method involves the use of matrix solid-phase dispersion (MSPD) prior to their determination by gas chromatography – electron-capture negative ion mass spectrometry (GC-ECNI-MS) operating in the selected-ion-monitoring (SIM) mode. The parameters affecting the extraction efficiency of the target analytes from biota sample were optimized using a Box-Behnken design method. The optimal extraction conditions involved dispersing of freeze-dried biota sample (1 g) with 2 g of silica gel in a glass tube by a vigorous shaking (1.0 min) to obtain a dry homogenous mixture. This mixture was transferred to a glass column containing 1 g of Florisil, as the clean-up co-sorbent. The target analytes were then eluted with 20 mL of n-hexane. The extract was adjusted to 1 μL and then determined by GC-ECNI-MS. The limits of detection (LODs) were 0.6 ? 2 pg/g. A preliminary result revealed that trace levels of chlorinated flame retardants were detected in various biota samples.
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