博碩士論文 102326007 詳細資訊



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姓名 詹凱博(Kai-Po Chan)  查詢紙本館藏   畢業系所 環境工程研究所
論文名稱 氣相層析三段四極柱串聯質譜儀應用於多溴二苯醚環境樣品之分析
(Application of Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry (GC/MS-QqQ-MS) for the Analysis of Polybrominated Diphenyl Ethers (PBDEs))
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摘要(中) 目前市面上微量濃度的多溴二苯醚（Polybrominated diphenyl ethers, PBDEs）樣品檢測仍多依賴氣相層析/高解析質譜儀（Gas chromatography /High resolution mass spectrometer, GC/HRMS）系統，主要乃因其具有絕佳的精密度與偵測極限等優點。然而，此套設備不僅購置費用昂貴且體積龐大外，在操作維護的難度及成本也極高，因此國內能夠擁有HRMS且具備超微量PBDEs多種同源物定量能力的實驗室並不多見，形成技術推廣上的一大瓶頸。相較於GC/HRMS的這些限制，氣相層析/串聯式質譜儀（GC-MS/MS）由於近年來在感度上已大幅提升，加上具有相對低廉的價格、較小的佔用空間、較易維護及較低分析成本等優點，歐盟於2014年將此系統與GC/HRMS列為在戴奧辛檢測分析上具有同等級的確認方法，因此極有潛力在未來能成為檢測PBDEs的新方法。本研究即嘗試以新型氣相層析/串聯式質譜儀（Thermo TSQ 8000 Evo）建置PBDEs分析方法，建置規範參考歐盟Commission Regulation （EU）No 589/2014及環檢所公告方法NIEA M802.00B，使用的管柱為DB-5HT （Length：15m，I.D.：0.25mm，Film：0.1μm），分析時間為24分鐘，PBDEs建置的種類共27種（一至十溴），以5組標準品溶液建立檢量線，其感應因子（RRF）之相對標準偏差RSD (%)除BDE-156與BDE-196（分別21.1%與24.7%）外均於20%以下，同時其具有良好的線性關係(R2>0.998)、優異的偵測極限、精密度與準確度，在檢測不同環境基質樣品中多種PBDEs微量濃度(ppt及ppq等級)的表現上，GC-MS/MS檢測結果與HRMS僅呈現出20%系統性負偏差，因此未來具有廣泛的應用前景。
摘要(英) To date, trace levels of polybrominated diphenyl ethers (PBDEs) in environmental samples have been primarily measured using the gas chromatography/high resolution mass spectrometer (GC/HRMS) system. While GC/HRMS systems have many advantages such as excellent precision and detection limits, they also have several major bottlenecks for technology promotion including expensive acquisition, costly operation and maintenance, as well as bulky volume, resulting in only few laboratories in Taiwan that have the capacity to perform PBDEs analysis with GC/HRMS systems. Nonetheless, due to its substantial sensitivity improvement, the gas chromatography/tandem mass spectrometry (GC-MS/MS) system has draw a great deal of attention lately and is considered potentially to be used as a confirmatory method for PBDEs in the future. In fact, the GC-MS/MS system has been included in the regulations of the European Union on analysis for the official control of dioxin levels in 2014. The major reasons for it are, in contrast to these restrictions of GC/HRMS systems, that they are cheaper to acquire and operate, easier to maintain, and have a relatively compact size. In this study, we aimed to develope an analytic method for PBDEs by the use of Thermo Scientific™ TSQ™ 8000 Evo system and its establishment specification is referencing European Commission Regulation (EU) No 589/2014 and NIEA M802.00B, which is announced by Environmental Analysis Laboratory, Taiwan. The total 27 congeners of PBDEs established convering one to ten bromine moieties that were tested by the following settings: DB-5HT column (Length: 15m, I.D.: 0.25mm and Film: 0.1μm), 24 minutes as analysis period, and the calibration curve was prepared using five groups of standard solution. The results show that most of their Relative Response Factor of the relative standard deviation were less than 20%, except BDE-156 and BDE-196 that were 21.1% and 24.7%, respectively. Moreover, these results were obtained in good linearity (R2> 0.998), excellent detection limits, precision and accuracy. Our results suggest that the GC-MS/MS system has broad application prospects for the detection of trace PBDEs among diverse environmental matrices due to that performance achieves merely 20% negative systemic deviation in comparison with GC/HRMS systems (at both ppt and ppq levels).
關鍵字(中) ★ 多溴二苯醚
★ 氣相層析/串聯式質譜儀
★ 氣相層析儀/高解析質譜儀		 關鍵字(英) ★ PBDEs
★ GC-MS/MS
★ GC/HRMS
論文目次 摘要 i
Abstract ii
致謝 iv
目錄 v
圖目錄 vii
表目錄 xi
第一章 前言 1
1.1 研究緣起 1
1.2 研究目的 2
第二章 文獻回顧 3
2.1 持久性有機污染物 3
2.2 多溴二苯醚 4
2.2.1 多溴二苯醚之基本特性 6
2.2.2 多溴二苯醚於環境中之流布 8
2.2.3 多溴二苯之管制策略 12
2.3 傳統檢測技術儀器 14
2.3.1 質譜儀(Mass spectrometer，MS) 15
2.3.2 電子捕獲器(ECD、μECD) 21
2.4 近代檢測技術儀器 22
2.4.1 串聯式質譜儀(Tandem Mass Spectrometry, MS/MS) 24
2.5 氣相層析三段四極柱串聯質譜儀(GC/MS-QqQ-MS) 26
第三章 研究方法 29
3.1 研究流程設計 29
3.2 實驗藥品與試劑 29
3.2.1 實驗藥品 29
3.2.2 實驗溶劑 29
3.3 實驗材料與設備 30
3.3.1 實驗材料 30
3.3.2 實驗設備 31
3.4 檢量線建置 32
3.4.1 PBDEs標準品 32
3.4.2 相對感應因子(Relative Response Factor,RRF) 36
3.5 氣相層析三段四極柱串聯質譜儀(GC/MS-QqQ-MS)設定 37
3.5.1 氣相層析(GC) 37
3.5.2 三段四極柱(Triple Quadrupole,QqQ)質譜儀 37
3.5.3 母離子、子離子對測試 37
3.5.4 解析度測試 38
3.6 高解析度氣相層析/高解析度質譜儀設定 40
3.6.1 高解析度氣相層析(HRGC) 40
3.6.2 高解析度氣質譜儀(HRMS) 40
3.6.3 監測離子及質荷比設定 40
3.7 準確度與精密度評估 44
3.7.1 儀器之準確度與精密度 44
3.7.2 方法之準確度與精密度 45
3.8 方法之偵測極限評估 45
3.9 真實樣品分析 46
3.9.1 樣品萃取與淨化 46
3.10 品保品管 48
3.10.1 內標準品回收百分率 48
3.10.2 空白基質添加待測物標準品回收率 48
3.10.3 檢量線確認標準品回收率及相對標準偏差 48
第四章 結果與討論 49
4.1 串聯質譜儀之最適分析條件 49
4.1.1 母離子、子離子與碰撞能量 49
4.1.2 解析度之探討 62
4.2 方法之偵測極限評估 64
4.3 線性範圍之討論 68
4.4 準確度與精密度評估 70
4.4.1 儀器之準確度與精密度 70
4.4.2 方法之準確度與精密度 73
4.5 真實樣品分析 75
4.5.1 底泥樣品 75
4.5.2 生物體(魚體)樣品 80
4.5.1 水體樣品 85
4.6 品保品管 90
4.6.1 內標準品回收率 90
4.6.2 空白基質添加待測物標準品回收率 99
第五章 結論與建議 102
5.1 結論 102
5.2 建議 103
參考資料 104
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指導教授 林居慶(Chu-Ching Lin) 審核日期 2016-7-20
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