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样品经乙腈提取后,用无水硫酸钠柱净化,正己烷脱脂,乙酸乙酯液液萃取,再经旋转蒸发仪浓缩后,用流动相定容,紫外检测器254 nm波长检测,外标法定量。结果表明,用优化改进后的方法测定的甲基睾酮残留量,回收率为78.5%~86.5%,优于中国水产行业标准SC/T 3029——2006《水产品中甲基睾酮残留量的测定》。改进后的前处理比较符合实验室实际操作,准确可靠、快速简便,明显提高了工作效率,是一种适用于批量样品同时测定水产品中甲基睾酮残留量的高效液相色谱方法。
After the sample was extracted with acetonitrile, the residue was purified by anhydrous sodium sulfate column, defatted with n-hexane, liquid-liquid extraction with ethyl acetate and concentrated by rotary evaporator. The mobile phase was fixed with a UV detection 254 nm wavelength detector. Quantitative. The results showed that the methyltestosterone residue was recovered from 78.5% to 86.5% with the optimized and improved method, which was better than the determination of methyltestosterone residues in aquatic products of China Aquaculture Industry Standard SC / T 3029-2006 ". The improved pretreatment is in line with the actual laboratory operation, accurate and reliable, quick and easy, and obviously improves the working efficiency. It is a high performance liquid chromatographic method suitable for the simultaneous determination of methyltestosterone residues in aquatic products in batch samples.