以微波輔助萃取搭配氣相層析質譜儀檢測底泥樣品中有機磷耐燃劑之研究; Determination of Organophosphate Flame retardants in Sediment by Microwave-Assisted Extraction and Gas Chromatography Mass Spectrometry

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题名:	以微波輔助萃取搭配氣相層析質譜儀檢測底泥樣品中有機磷耐燃劑之研究;Determination of Organophosphate Flame retardants in Sediment by Microwave-Assisted Extraction and Gas Chromatography Mass Spectrometry
作者:	鍾孝武;Siao-Wu Jhong
贡献者:	化學研究所
关键词:	氣相層析質譜儀;微波輔助萃取;氣相層析儀;耐燃劑;有機磷耐燃劑;GC-MS;GC;Gas Chromatography Mass Spectrometry;MAE;OPFR;Flame retardants;Microwave-Assisted Extraction;Organophosphate Flame retardants
日期:	2009-06-18
上传时间:	2009-09-22 10:21:00 (UTC+8)
出版者:	國立中央大學圖書館
摘要:	有機磷耐燃劑(Organophosphate flame retardants, OPFRs)被廣泛的用於各種材料之中，如：PVC塑料、PU塑料、油漆塗料、壁紙、紡織品、電子產品等。在2004年全世界的有機磷耐燃劑用量達30萬噸以上。相較於溴系耐燃劑(如：Polybrominated diphenyl ethers，PBDEs、Hexabromocyclododecane，HBCDs)，有機磷耐燃劑具有較佳的水溶性，因此其被認為更具有移動性，較容易藉由水路徑而進入到環境之中。有機磷耐燃劑相較於溴系耐燃劑被認為其毒性較低，同時對環境的傷害也較小。但部分有機磷耐燃劑，如三-(2-氯乙基)磷酸酯{Tris-(2-chloroethyl)phosphate, TCEP}被國際癌症研究機構(International Agency for Research on Cancer, IARC)判定為第三類的致癌物(Group 3 carcinogen)。因有機磷耐燃劑如此廣泛的被使用於生活之中，故我們有所必要發展一個快速且便利的方法以偵測環境中的有機磷耐燃劑。本研究發展了一個以微波輔助萃取(microwave-assisted extraction,MAE)結合氣相層析質譜儀(GC-MS)偵測底泥樣品中五種常用有機磷耐燃劑的檢測方法。於此將有機磷耐燃劑運用微波輔助萃取的各項參數(如：萃取溶劑種類與體積、萃取溫度、萃取時間等)，作一系統性的研究並將參數最佳化。微波輔助萃取法所得之最佳化實驗參數如下，以40 mL的丙酮作為萃取溶劑，在120℃下對2 g的底泥樣品進行20分鐘的萃取。後利用HLB固相萃取管柱與氧化鋁以淨化萃取液。本實驗的定量極限(limits of quantification, LOQ)可達100-250 pg/g(乾重)。除利用GC-EI-MS以選擇離子偵測模式定量外，並利用GC-CI-MS以定性。本實驗的萃取回收率在60-106%之間，相對標準偏差在1-11%之間。與文獻中的其他萃取方法相較之下，本實驗有著更良好的結果。最後將本方法應用於真實底泥樣品中，各樣品的有機磷耐燃劑總濃度介於9-13 ng/g之間。 Organophosphate flame retardants (OPFRs) have been used widely in a large variety of materials, such as PVC plastics, polyurethane foams, paints, wall papers, textiles, and electronic equipment, etc. In 2004, more than 300,000 tons of OPFRs were used worldwide. Because OPFRs were more water-soluble than the brominated flame retardants (i.e., Polybrominated diphenyl ethers, PBDEs or Hexabromocyclododecane, HBCDs), OPFRs are assessed to be more mobile, so they are easier into environment by aquatic pathway. They are considered less toxicity and less harm to environment than brominated flame retardants, however, some OPFRs, such as TCEP, were classified by IARC as a Group 3 carcinogen. The widespread use of OPFRs and increasing public concern stimulated our interest in developing a rapid and reliable method for determining their presence and fate in aquatic environments. In this study, a microwave-assisted extraction (MAE) method coupled with gas chromatography-mass spectrometry (GC-MS) to determine five commonly used organophosphate flame retardants in sediment was presented. Parameters such as type and volume of extraction solvent, extraction temperature, time for the quantitative extraction of OPFRs by MAE were optimized. The OPFRs can be completely extracted by 40 mL acetone at 120 °C with 20 min of extraction from 2 g sediment sample. HLB-SPE coupled with aluminium oxide was employed to cleanup the extract. Limits of quantification (LOQs) were established between 100 to 250 pg/g (dry weight) for 2 g sediment sample. Moreover, GC-MS with chemical ionization was used to confirm the identification of the analytes. Recovery of OPFRs in spiked sediment samples ranged from 60% to 106% with 1-11% RSD. The results obtained using this approach is better than that from the previous reported methods. This developed method was finally applied to real sediment samples, a preliminary result shows that their total concentrations were ranging from 9 to 13 ng/g.
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