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建立了超高压液相色谱法测定水产品中甲基睾酮残留量的方法。样品采用乙酸乙酯超声波提取,石油醚去脂,乙酸乙酯反萃取,旋转蒸发后用流动相溶解残渣,过滤后上机分析。以V(甲醇):V(水)=60:40为流动相,以C18柱(2.1 mm×100 mm,1.7μm)为色谱分离柱在254nm波长进行测定。方法在5.0~250 ng/mL范围内线性良好(R2=0.9997),在5,30和100μg/kg添加水平下,方法回收率大于91%,相对标准偏差小于7%,定量限为5μg/kg。
A method for the determination of methyltestosterone in aquatic products by ultra-high pressure liquid chromatography was established. The samples were extracted with ethyl acetate, extracted with petroleum ether, reextracted with ethyl acetate. The residue was purified by mobile phase after rotary evaporation. After filtration, the samples were analyzed on the machine. The mobile phase was V (methanol): V (water) = 60:40, and the column was C18 (2.1 mm × 100 mm, 1.7 μm). The method was linear in the range of 5.0-250 ng / mL (R2 = 0.9997). The method recoveries were more than 91% at RSD of 5, 30 and 100 μg / kg with the relative standard deviation less than 7% and the limit of quantification was 5 μg / kg .