以高效液相層析法分析豬肉、牛肉及豬肝中動物用藥Clenbuterol   全文下載

High Performance Liquid Chromatography to Determine Animal Drug Clenbuterol in Pork, Beef and Hog Liver

以半微量高效液相層析儀（semi-micro HPLC）分析clenbuterol 在豬肉, 牛肉和豬肝中之含量。檢體經0.4 N過氯酸均質萃取，取上清液以乙醚液液萃取淨化後濃縮，再以0.2 N硫酸定容，HPLC使用之層析管柱為Waters Cosmosil 5C18-MS（2.0×150 mm），移動相為0.05 M NaH2PO4（pH3.0）/acetonitrile（80/20，v/v），以紫外光檢出器波長212 nm檢測。分別添加0.0005~0.01 ppm之clenbuterol於豬肉、豬肝及牛肉檢體中進行回收試驗，其回收率達80.9~90.6%。本研究建立之方法在此三種檢體中之最低檢出限量為0.0001 ppm， 此結果均能達到聯合國世界糧農組織/世界衛生組織（FAO/WHO）之食品添加物規格委員會（JECFA）及我國衛生署於2001年所規定之「動物用藥殘留標準」中容許此藥劑之殘留量在牛之肝、腎中0.0006 ppm及牛肉中0.0002 ppm之檢測。利用此檢驗方法分析市售豬肉、豬肝及牛肉中c l e n b u t e r o l 之殘留量，檢體共計150 件，殘留量範圍在0.0001~0.00015 ppm，並未超過衛生署之限量標準。"

A semi-micro high performance liquid chromatography (HPLC) was developed to determine clenbuterol in pork, beef and hog liver. The procedure included extraction with 0.4 N perchloric acid, partitionally separation with diethyl ether, and then back-extraction with 0.2 M sulphuric acid. Analytical procedure was performed by HPLC with a Waters Cosmosil column 5C18-MS (2.0 × 150 mm), a mobile phase of 0.05 M NaH2PO4 (pH3.0)/acetonitrile solution (80/20, v/v) and absorbance at 212 nm. The recoveries of clenbuterol in pork, beef and hog liver spiked with standards of 0.0005~0.01 ppm were 80.9~90.6 %. The detection limit of clenbuterol in tested samples was 0.0001 ppm, which is lower than the officially allowed level. The equation was linear for detecting 0.0002~0.001 ppm clenbuterol. The method was validated to be usable for market samples. Three out of 150 samples were detected to contain clenbuterol (0.0001~0.00015 ppm), which were less than both JECFA and Department of Health regulation levels (hog liver 0.0006 ppm and beef 0.0002 ppm).