雞肉及雞肝中動物用藥安保寧(amprolium)殘留量檢驗方法之探討   全文下載

Determination of Amprolium Residue in Chicken Meat and Liver

本研究利用後置反應及螢光檢測之高效液相層析法建立雞肉及雞肝中動物用藥安保寧（amprolium）殘留量之檢驗方法。雞肉及雞肝檢體以乙?萃取，經過濾，濃縮，去除雜質後，與離子配對試劑二辛基硫琥珀酸（dioctyl sulfosuccinate; DOSS）形成複合物，以二氯甲烷抽提，其中雞肝檢體須進一步以Sep-Pak酸性氧化鋁處理匣淨化，最後利用高效液相層析儀將安保寧先以Cosmosil 5C18-AR-II(25 cm×4.6 mm i. d., 5 μm)管柱分離，再與鐵氰化鉀之氫氧化鈉溶液反應，以螢光檢測器於激發波長368 nm及放射波長470 nm偵測。檢體中添加安保寧0.05、0.1及0.2 ppm時，其回收率於雞肉及雞肝中分別為95.8~98.3%及91.3~95.2%，變異係數皆小於2%。本方法在此二檢體中之檢出限量為5 ppb。將此方法應用於市售雞肉及雞肝之殘留量分析，結果於50件檢體中檢出1件雞肝殘留安保寧0.04 ppm，檢出率占總抽驗件數之2%。"

A high performance liquid chromatographic (HPLC) method using postcolumn reaction and fluorometric detection was evaluated for the determination of amprolium in chicken meat and liver. Amprolium was extracted with acetonitrile and filtered. The extract was evaporated to dryness and partitioned with n-hexane and dichloromethane. An ion-pair complex with an anionic surfactant, dioctyl sulfosuccinate (DOSS), was formed. The ion-pair complex was extracted with dichloromethane and evaporated to dryness. The residue from chicken liver was cleaned up using a Sep-Pak alumina A cartridge before it was quantitatively analyzed by HPLC. Amprolium was separated by HPLC on a column of Cosmosil 5C18-AR-II (25 cm×4.6 mm i. d., 5 μm), reacted with potassium ferricyanide in a postcolumn reaction system, and determined by a fluorescence detector with excitation at 368 nm and emission at 470 nm. The average recoveries of amprolium after spiking into samples at the levels of 0.05, 0.1 and 0.2 ppm were in the ranges of 95.8-98.3% for meat and 91.3-95.2% for liver. The coefficients of variation were less than 2%. The detection limit was 5 ppb.Twenty-five samples each of chicken meat and liver were purchased from various markets in Taipei during March-June, 1997. Only one chicken liver sample was found to have 0.04 ppm amprolium residue. The percentage of detection was 2%.