Chu Pak-Sin, Lopez Mayda, Serfling Stan, Gieseker Charlie, Reimschuessel Renate
Center for Veterinary Medicine, U.S. Food and Drug Administration, Laurel, Maryland 20708, USA.
J Agric Food Chem. 2006 May 3;54(9):3193-8. doi: 10.1021/jf052701r.
An analytical method was developed to quantitate and confirm the presence of 17alpha-methyltestosterone in the muscles of tilapia, rainbow trout, and salmon. The method employed two liquid-liquid partitioning steps and two solid-phase extraction columns for sample cleanup. The final extracts were analyzed on an isocratic reverse-phase liquid chromatography-tandem mass spectrometry system with atmospheric-pressure chemical ionization in the positive ion mode. The method was validated at levels from 0.40 to 1.6 ng/g, with MT-d3 used as an internal standard. The accuracy was between 100% and 110%, and coefficients of variation of <10% were obtained for all three fish species. Muscle tissues from dosed fish were also assayed to demonstrate the effectiveness of the method for recovering the parent drug.
开发了一种分析方法，用于定量和确认罗非鱼、虹鳟鱼和鲑鱼肌肉中17α-甲基睾酮的存在。该方法采用两步液液分配和两根固相萃取柱进行样品净化。最终提取物在等度反相液相色谱-串联质谱系统上进行分析，采用大气压化学电离正离子模式。该方法在0.40至1.6 ng/g的水平上进行了验证，使用MT-d3作为内标。准确度在100%至110%之间，三种鱼类的变异系数均小于10%。还对给药鱼的肌肉组织进行了检测，以证明该方法回收母体药物的有效性。
