超高液相色谱-串联质谱法测定淡水水产动物中6种激素残留

Determination of 6 kinds of hormone residues in freshwater aquatic animals by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超声提取  凝胶净化色谱  超高液相色谱-串联质谱法  水产动物  激素

英文关键词:ultrasonic extraction  gel permeation chromatography  ultra performance liquid chromatography- tandem mass spectrometry  aquatic animals  hormone

中文摘要:

      目的 建立超声提取-凝胶净化色谱(gel permeation chromatography, GPC)-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测淡水水产动物中的雌酮、炔诺酮、炔雌醇、米非司酮、己烯雌酚和己酸羟孕酮残留量的方法。方法 取淡水水产动物可食部分粉碎后, 准确称取5.0 g, 置于50 mL离心管中, 加甲醇超声提取, 放冷, 8000 r/min离心5 min。离心后的溶液净化后, 氮吹至近干, 残渣加甲醇溶解, 过滤后上UPLC-MS/MS进行定性、定量检测。结果 各组分在0.01~10.00 μg/mL范围内线性关系良好, 相关系数均大于0.995; 检出限为0.121~0.285 μg/kg, 定量限为0.363~0.855 μg/kg; 加标回收率均在80.0%~110.0%范围内; 重复性相对标准偏差均在5.0%以内(n=6)。结论 方法专属性好、灵敏度高, 适用于淡水水产动物中极微量激素残留的检测。

英文摘要:

      Objective To establish a method for the determination of estrone, norethindrone, ethinylestradiol, mifepristone, diethylstilbestrol and hydroxyprogesterone caproate residues in freshwater aquatic animals by ultrasonic extraction-gel permeation chromatography (GPC) purification-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After the edible part of fresh water aquatic animals was crushed, 5.0 g was weighed accurately and put into a 50 mL centrifugal pipe, added with methanol ultrasonic extraction. After cooling, it was centrifuged for 5 min at 8000 r/min. After the centrifuged solution was purified, it was blown to near dry by nitrogen. The residue was dissolved with methanol, and then it was qualitative and quantitative tested by UPLC MS/MS after filtration. Results Each component had a good linear relationship in the range of 0.01?10.00 μg/mL, and the correlation coefficients were greater than 0.995. The limits of detection were 0.121?0.285 μg/kg. The limits of quantitation were 0.363?0.855 μg/kg. The recoveries were in the range of 80.0%?110.0%. The relative standard deviation of repeatability was within 5.0% (n=6). Conclusion The method is of good specificity and high sensitivity, which is suitable for the detection of trace hormone residues in freshwater aquatic animals.