牛肉及牛肝中Trenbolone及其代謝物之檢驗方法   全文下載

A Method for the Determination of Trenbolone in Bovine Muscle and Liver

利用高效液相層析建立牛肉中trenbolone acetate及其代謝產物17α-trenbolone （17α-TBOH）及17β-trenbolone （17β-TBOH）殘留量之檢驗方法。牛肉以乙?萃取，經過濾、以乙?飽和之正己完去除脂溶性雜質及濃縮後，再以Bond Elut C18過濾層析匣淨化，最後利用高效液相層析法進行分析。層析條件為層析管柱Inertsil ODS-3V 5μrn （4.6 i.d. × 250 mm），移動相為乙?／甲醇／水（50：10：40，v／v）溶液，流速1 mL／min，以紫外光波長340 nm偵測。牛肉樣品中添加trenbolone acetate、17α-trenbolone及17β-trenbolone各2~4 ppb時，其回收率為83.8~98.9%牛肝中添加trenbolone acetate、17α-trenbolone及17β-trenbolone各10~20 ppb時，其回收率為82.6~95.7%。本方法對牛肉中17α-trenbolone及17β-trenbolone之最低檢出極限均為0.5 ppb，對牛肝則均為2 ppb，對牛肉中trenbolone acetate之最低檢出極限為1 ppb，對牛肝則為4 ppb。以此方法檢驗市售牛肉檢體30件，結果均低於最低檢出限量。

A high performance liquid chromatographic (HPLC) method was developed for the determination of trenbolone acetate, 17α-trenbolone and 17β-trenbolone in bovine muscle and liver. Bovine muscle sample was extracted with acetonitrile, filtered, and defatted with acetonitrile-saturated n-hexane. The acetonitrile extract after concentration and clean-up with Bond Elut C18 cartridge was ready for HPLC analysis. HPLC conditions were as follows, column: Inertsil ODS-3V, mobile phase: acetonitrile/methanol/H2O (50:10:40, v/v), flow rate: 1 mL/min, and detecting wavelength: UV 340 nm. For bovine muscle, the recoveries were 83.8~98.9% for trenbolone acetate, 17α-trenbolone and 17β-trenbolone spiked at concentrations between 2~4 ppb, and the variation coefficients were 1.2~4.8%. For bovine liver, the recoveries were 82.6~95.7% for the three trenbolones spiked at concentrations between 10~20 ppb, and the variation coefficients were 1.9~6.7%. The detection limits for trenbolone acetate, 17α-trenbolone and 17β-trenbolone were 1, 0.5 and 0.5 ppb in bovine muscle, and 4, 2 and 2 ppb in bovine liver, respectively. After the survey, 30 marketed bovine muscle samples showed no detection of trenbolone acetate and its metabolites.