食品中全氟及多氟烷基化合物分析方法開發   全文下載

Development of an Analytical Method for Per- and Polyfluoroalkyl Substances in Foods

全氟與多氟烷基化合物（Per- and polyfluoroalkyl substances, PFAS）因其高穩定性及疏水疏油等特性，廣泛應用於各行業，但因其難以分解，具有生物累積之風險，歐洲食品安全局於2020年提出這些物質會影響發育，以及可能對血清膽固醇、肝臟及免疫系統等造成不利影響，並提出每週耐受攝取量為PFOA、PFNA、PFHxS及PFOS之總和4.4 ng/kg bw/wk。隨著國際對食品中PFAS規範趨嚴，歐盟亦於2023年訂定上述4品項個別及總和之限量標準，個別限量範圍介於0.2-50μg/kg，總和限量範圍介於1.3-50μg/kg。本研究針對魚類、肉類、蛋類、奶類及食用內臟類基質建立以QuEChERS前處理技術及使用EMR lipid固相萃取匣淨化流程，並利用遲滯管排除系統背景干擾，以液相層析串聯質譜儀分析食品中19項PFAS之方法。由添加回收試驗結果顯示，平均回收率及變異係數於魚類介於77.2-97.9%及2.8-16.3%；蛋類介於73.7-91.1%及4.6-18.3%；牛奶介於63.7-97.7%及3.2-14.9%；豬肉介於71.7-96.3%及3.3-15.1%；內臟類介於70.0-106.0%及2.7-20.6%，上述結果皆符合衛生福利部食品藥物管理署「食品化學檢驗方法之確效規範」。本方法之定量極限介於0.02-0.25μg/kg，標準曲線之線性範圍為0.005-0.5 ng/mL，r值為0.99以上，線性關係良好。本方法靈敏、穩定、適用多種食品基質且具有良好的準確性及精密度，可供各界參考使用。

Per- and polyfluoroalkyl substances (PFAS) are widely used across industries due to their exceptional stability as well as hydrophobic and oleophobic properties. However, these compounds are highly persistent to decompose which carrying risk of bioaccumulation. The European Food Safety Authority (EFSA) proposed in 2020 that PFAS may cause developmental effects and adverse impacts on serum cholesterol, liver function and immune system. EFSA proposed a tolerable weekly intake (TWI) of 4.4 ng/kg body weight/week for the combined exposure to PFOA, PFNA, PFHxS and PFOS. The European Union set the maximum levels for PFAS in food stuffs in 2023. 0.2 to 50μg/kg for individual PFAS and 1.3 to 50μg/kg for the sum of the four regulated compounds. This study established a method for the determination of 19 PFAS in fish, meat, eggs, milk, and edible offal. The approach combined QuEChERS pretreatment, an EMR lipid solid-phase extraction cartridge, and a delay column to eliminate background interference from the analytical system in liquid chromatograph-tandem mass spectrometry (LC-MS/MS) analysis. The results of the spiking tests showed that the average recoveries of 19 PFAS in fish were 77.2-97.9% with the coefficients of variation of 2.8-16.3%; those in eggs were 73.7-91.1% with the coefficients of variation of 4.6-18.3%; those in milk were 63.7-97.7% with the coefficients of variation of 3.2-14.9%; those in meat were 71.7-96.3% with the coefficients of variation of 3.3-15.1%; those in edible offal were 70.0-102.2% with the coefficients of variation of 2.7-20.6%. All results met the“Validation guideline of the food chemical testing method”published by the Taiwan Food and Drug Administration. The limits of quantification were 0.02-0.25μg/kg, and the linear range of the standard calibration curves calibrated by the internal standards were 0.005-0.5 ng/mL with the coefficients of correlation higher than 0.99. The developed method is sensitive, stable, suitable for various applications across diverse food matrices, offering good accuracy and precision suitable forroutine momitoring and public helath protection.