以液相層析串聯式質譜儀測定硝基呋喃及其代謝物在魚組織中分析方法之研究   全文下載

Quantitative Determination of Four Nitrofurans and Corresponding Metabolites in the Fish Muscle by Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry

本研究著重於以液相層析串聯式質譜儀法分析硝基?喃劑及其代謝物，同時萃取多種藥物的方法開發，包括富來頓（Furazolidone）、富來他頓（Furaltadone）、硝化富樂遜（Nitrofurazone）和硝化富蘭音（Nitrofurantoin）與其對應之代謝物 AOZ 、AMOZ 、SC和AH，方法確效根據歐盟法規所規範之確效參數；樣品是先以鹽酸水解後加入2-nitro-benzaldehyde衍生，再以乙酸乙酯萃取，以氮氣濃縮乾燥後加入50% 甲醇溶液回溶，最後以LC-ESI-MS/MS分析。本研究結果發現此4種硝基?喃劑及其代謝物的偵測極限分別為10 μg/kg與1.0 μg/kg，決策極限（CCα）分別為2.93-5.01 μg/kg和0.19-0.43 μg/kg，而偵測能力（CCβ）則分別為3.62-6.20 μg/kg與0.23-0.54 μg/kg，此外本分析方法檢量線之有效線性濃度分別為1.0-100 μg/kg與0.1-10.0 μg/kg。

A method validated based on the European Union (EU) regulations for determining the presence of furazolidone, furaltadone, nitrofurazone, nitrofurantoin and their corresponding metabolites AOZ, AMOZ, SC and AH in fish muscle was developed. Samples were acid-hydrolyzed, treated with 2-nitrobenzaldehyde and extracted with ethyl acetate. The extracts were dried in a N2 stream and redissolved in methanol:water (50:50, v/v). Analysis was performed by LC/ESI/MS/MS. This developed method carried limits of quantification lower than 10 μg/kg for the nitrofurans and 1.0 μg/kg for the metabolites. It was observed that the decision limit (CCα) ranged from 2.93 to 5.01 μg/kg for the nitrofurans and 0.19 to 0.43 μg/kg for the metabolites. The detection capability (CCβ) was between 3.62 and 6.20 μg/kg for the nitrofurans and between 0.23 and 0.54 μg/kg for the metabolites. The linear calibration curve parameters in the fortified fish muscle were between 1.0-100.0 μg/kg and 0.1-10.0 μg/kg for the nitrofurans and metabolites, respectively.