利用基質固相萃取技術及HPLC分析畜產品中動物用藥Febantel、Fenbendazole、Oxfend azole及Oxfendazole Sulfone   全文下載

Simultaneous Determination of Febantel, Fenbendazole, Oxfendazole and Oxfendazole Sulfone in Livestock by Matrix Solid Phase Dispersion Extraction Technique and HPLC

本研究分別探討以傳統及基質固相分散（matrix solid phase dispersion, MSPD）方法萃取畜產品中fehantel、fenhendazole、oxfendazole及oxfendazole sulfone四種動物用藥，再利用高效液相層析法（high performance liquid chromatography, HPLC）配合光二極體列陣檢出器（photodiode array detector, PDAD）分析。傳統方法係將檢體中之動物用藥在鹼性情況下以乙?萃取，經Sep-Pak C18萃取匣淨化後，再以HPLC／PDAD分析。MSPD技術則將檢體與Bondesil-C18混合後充填於管柱中，再與中性氧化鋁萃取匣串聯，並以乙?沖提，再以HPLC／PDAD檢測。兩種方法分別添加三種濃度之動物用藥，傳統方法除fehantel因操作過程部分會轉換，以致回收率介於72.3-81.6%，及低濃度（0.04 ppm）之fenhendazole回收率介於75.0-88.3%外，其餘濃度之動物用藥回收率介於80.3-108.7%之間，同日內及異日間之變異係數分別小於6.95%及12.12%。MSPD方法之回收率介於80.2-109.6%之間，同日內及異日間之變異係數分別小於4.47%及7.89%。傳統方法之最低檢出限量介於0.010~0.020 ppm，MSPD方法則介於0.025~0.050 ppm。MSPD方法回收率佳，操作簡便，並可縮短分析時間，節省溶劑，較利於例行性之檢驗工作。"

Febantel, fenbendazole, oxfendazole and oxfendazole sulfone in livestock products were simultaneously extracted by traditional and matrix solid phase dispersion (MSPD) method, and then analyzed by high performance liquid chromatography (HPLC). In the traditional method, four benzimidazoles were extracted with acetonitrile under basic conditions, partitioned with n-hexane, and cleaned by a Sep-Pak C18 cartridge. In the MSPD method, samples were blended with Bondesil-C18, and the mixture was packed in a filtration column. This column was connected in tandem with an alumina N cartridge and eluted with acetonitrile. These benzimidazoles were determined by HPLC with a photodiode array detector. Recovery tests of benzimidazoles by these two methods were performed at three spike levels. In the traditional method, febantel was found to be unstable during the sample preparation. Average recoveries of febantel ranged from 72.3 to 81.6%. Average recoveries at low concentration (0.04 ppm) of fenbendazole ranged from 75.0 to 88.3%, while the remaining benzimidazoles ranged from 80.3 to 108.7%. The coefficients of variation of intra-day and inter-day assays were lower than 6.95 and 12.12%, respectively. Average recoveries of the MSPD method ranged from 80.2 to 109.6%. The coefficients of variation of intra-day and inter-day assays were lower than 4.47 and 7.89%, respectively. The detection limits for benzimidazoles were 0.010~0.020 ppm for the traditional method and 0.025~0.050 ppm for the MSPD method. The MSPD method minimized sample preparation time and solvents, and the analyte was stable during the analytical procedure with high recoveries. The MSPD method is suggested for use in routine analysis of benzimidazoles in livestock products. 本研究分別探討以傳統及基質固相分散（matrix solid phase dispersion, MSPD）方法萃取畜產品中fehantel、fenhendazole、oxfendazole及oxfendazole sulfone四種動物用藥，再利用高效液相層析法（high performance liquid chromatography, HPLC）配合光二極體列陣檢出器（photodiode array detector, PDAD）分析。傳統方法係將檢體中之動物用藥在鹼性情況下以乙腈萃取，經Sep-Pak C18萃取匣淨化後，再以HPLC／PDAD分析。MSPD技術則將檢體與Bondesil-C18混合後充填於管柱中，再與中性氧化鋁萃取匣串聯，並以乙腈沖提，再以HPLC／PDAD檢測。兩種方法分別添加三種濃度之動物用藥，傳統方法除fehantel因操作過程部分會轉換，以致回收率介於72.3-81.6%，及低濃度（0.04 ppm）之fenhendazole回收率介於75.0-88.3%外，其餘濃度之動物用藥回收率介於80.3-108.7%之間，同日內及異日間之變異係數分別小於6.95%及12.12%。MSPD方法之回收率介於80.2-109.6%之間，同日內及異日間之變異係數分別小於4.47%及7.89%。傳統方法之最低檢出限量介於0.010～0.020 ppm，MSPD方法則介於0.025～0.050 ppm。MSPD方法回收率佳，操作簡便，並可縮短分析時間，節省溶劑，較利於例行性之檢驗工作。