串聯質譜儀應用於食品中類戴奧辛化合物的快速檢測方法可行性探討

The feasibility study of using tandem mass spectrometer for rapid detection of dioxin-like compounds in food

陳思縈(Sz-Ying Chen)

指導教授 ： 蔡惠燕

中山醫學大學/健康管理學院/醫學應用化學系/碩士(2021年)

https://doi.org/10.6834/csmu202100209

摘要

戴奧辛呋喃及多氯聯苯化合物為環境中的持久性有機污染物，能透過食物鏈累積於人體脂肪組織，毒性作用強且會造成多種生理危害，在食品飼料中的容許限量值極低，為能達到超微量的檢測要求，在前處理流程及儀器分析步驟都有極嚴謹的品管規範，以致檢驗期程長達一週左右，往往在爆發食安事件之際，檢驗負荷遠超過實驗室量能，本研究目的在建立食品飼料中戴奧辛多氯聯苯的快速檢測方法。
首先導入氣相層析串聯質譜儀，確立分析參數及評估效能，再探討高溫加壓萃取油脂的較適化條件，並導入自動淨化系統以大幅縮短整體的分析期程，方法確效及實樣驗證，均以公告方法認證的分析程序，進行數值比對、統計檢定並提出完整的不確定度評估報告。
本研究建立的方法，適用於飼料、乳品、蛋品及大閘蟹等基質的戴奧辛呋喃、戴奧辛類多氯聯苯及指標性多氯聯苯分析，相較於現行公告方法7的認證實驗室系統，可大幅減少儀器建置費用、分析期程、溶劑用量及人力負擔，而回收率、精密度、樣品偵測極限皆符合公告方法的規範，，單一樣品在一天內可完成分析並取得結果，以真實樣品進行驗證比對，分析結果與認證流程分析結果無顯著差異，評估本方法的量測不確定度小於10%。

關鍵字

戴奧辛類化合物 ； 高壓溶劑萃取 ； 氣相層析串聯質譜儀 ； 不確定度評估

並列摘要

Dioxin furan and polychlorinated biphenyls (PCBs) are persistent environmental organic pollutants that can accumulate in human adipose tissue through the food chain. They are highly toxic and cause a variety of physiological hazards. Thus, the permissible limits in food and feed are extremely low. To meet the requirements of ultra-micro testing, the pretreatment process and the instrumental analysis procedures have strict quality control standards; thus, the testing period can last approximately one week. Unfortunately, the testing load often exceeds the laboratory capacity at the time of food safety incidents. Therefore, the objective of this study is to establish a rapid method for determining the amounts of dioxin polychlorinated biphenyls (PCBs) in food and feed. First, a gas chromatography-tandem mass spectrometer was used to determine the analytical parameters and evaluate the efficiency. The optimum conditions of high-temperature and high-pressure oil extraction were discussed, and an automatic purification system was introduced to considerably shorten the analysis period. The analytic procedure of the testing method verified the validity of the technique and the samples, and a complete evaluation report of the uncertainty was presented.
The method established in this study is suitable for analyzing dioxin furan, dioxin-type PCBs, and indicator PCBs in feed, dairy products, eggs, and hairy crabs. Compared with the certified laboratory system used in the current analytical method, this system can significantly reduce the cost of instrument construction, the analysis period, the solvent consumption, and the labor burden. Moreover, the recovery rate, precision, and sample detection limit are all in compliance with the standard specifications. A single sample can be analyzed, and results can be obtained in one day. After verification and comparison with actual samples, it was found that the analysis results were not significantly different from those of the existing certification process, and the measurement uncertainty of this method was estimated to be less than 10%.

並列關鍵字

Gas chromatography tandem mass spectrometer (GC/MS-MS) ； Dioxin like compound ； Non-dioxin-likePCBs (ICES- 6) ； Pressure solvent extraction(PSE) ； Measurement Uncertainty

參考文獻

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