本研究目標為建立一套以液相層析質譜儀精確地定性與定量動物檢體和環境水樣中perfluoropentanoic acid（PFPeA）、perfluorooctanoic acid（PFOA）、perfluorodecanoic acid（PFDA）、perfluorobutanesulfonate（PFBS）和perfluorooctanesulfonate（PFOS）等五種全氟界面活性劑之分析方法。液相層析儀動相是以甲醇和醋酸銨溶液組成。環境水樣前處理部份是以C18萃取管柱進行固相萃取法達到淨化濃縮目的；生物檢體前處理是以甲基第三丁基醚（MTBE）進行液-固相萃取法達到濃縮目的。實驗結果顯示PFPeA、PFBS、PFOA、PFOS和PFDA在水樣中的定量極限（LOQ）分別為6 ng/L、2 ng/L、2 ng/L、0.5 ng/L和2 ng/L。在14個不同環境水樣採樣點中，有11個採樣點被檢測到含有全氟界面活性劑，檢測率可高達79%，且PFOA、PFOS和PFDA被檢測最高總濃度可達到450 ng/L。動物檢體中PFPeA、PFBS、PFOA、PFOS和PFDA的定量極限分別為50 ng/g、20 ng/g、20 ng/g、5 ng/g和20 ng/g。動物檢體均可偵測到全氟界面活性劑，且PFOA、PFOS和PFDA被檢測最高總濃度可達到 1100 ng/g。 A method for the determination of perfluorooctanesulfonate (PFOS), perfluorooctanoate (PFOA) and perfluorodecanoate (PFDA) in various water and biological tissue samples was developed and validated in this study. The contents of PFCs in water samples were extracted by C18 solid-phase extraction (SPE). The biological tissue samples (frozen-dried fish and oysters) were simply extracted by liquid-solid extraction with MTBE and adding tetrabutylammonium hydrogensulfate (TBA) as an ion-pairing reagent. The analytes were then identified and quantitated by liquid chromatography-ion trap negative electrospray mass spectrometry (LC-ESI ion-trap-MS). Limits of quantitation (LOQ) were established between 0.5 to 6 ng/l in 250 ml of water sample, while 5 to 50 ng/g (dry weight) for biological tissue sample. Intrabatch and interbatch precision with their accuracy at two concentration levels were also investigated. Precision for these three PFCs, as indicated by RSD, proved to be less than 11 and 17%, respectively. The total contents of PFOA, PFOS and PFDA were detected in concentrations of up to 450 ng/l in various water samples, while up to 1100 ng/g in fish and oyster samples. PFOA and PFDA was the major PFCs detected in water samples and biological tissue samples, respectively.