建立罗非鱼肌肉中甲基睾丸酮残留量的超高效液相色谱-串联质谱联用(ultro high performance liquid chroma-tography-tandem mass spectrometry,UPLC-MS/MS)测定方法。以氘代试剂为内标,样品经乙腈萃取后,乙酸乙酯液液分配,强阴离子交...建立罗非鱼肌肉中甲基睾丸酮残留量的超高效液相色谱-串联质谱联用(ultro high performance liquid chroma-tography-tandem mass spectrometry,UPLC-MS/MS)测定方法。以氘代试剂为内标,样品经乙腈萃取后,乙酸乙酯液液分配,强阴离子交换柱净化,正己烷液液分离,硅酸镁固相萃取柱净化,采用UPLC-MS/MS选择离子监测(selected ion monitoring,SIR)正离子模式测定,可对罗非鱼肌肉中甲基睾丸酮残留进行定性和定量检测,检出限为0.4μg/kg,定量限为1μg/kg。线性范围为1～60μg/kg(r>0.999),方法的平均回收率范围为71.06%～83.06%,相对标准偏差为7.4%～15.3%。完全满足食品安全及进出口罗非鱼肌肉中甲基睾丸酮残留的监控和检测需要。展开更多
The use of synthetic anabolic steroid methyltestosterone (MT) as growth promoter is prohibited in China. Vali-dations of analytical methods for MT residue in food and the results obtained have become indispensable. Th...The use of synthetic anabolic steroid methyltestosterone (MT) as growth promoter is prohibited in China. Vali-dations of analytical methods for MT residue in food and the results obtained have become indispensable. The high perfor-mance liquid chromatography (HPLC) method for the detection of MT with liquid-liquid extraction by trichloromethane-methanol in carp muscle tissue was preliminarily validated with reference to the following parameters: recovery (accuracy)at the 1, 5 and 10mg kg-1 level, between-run and within-run CV values (repeatability, also called relative standard deviation(RSD)) and limit of detection. The recoveries were above 80% and the between-run and within-run CV values below 10%for muscle tissue. The limit of detection was 0.05 mg kg-1.展开更多
文摘建立罗非鱼肌肉中甲基睾丸酮残留量的超高效液相色谱-串联质谱联用(ultro high performance liquid chroma-tography-tandem mass spectrometry,UPLC-MS/MS)测定方法。以氘代试剂为内标,样品经乙腈萃取后,乙酸乙酯液液分配,强阴离子交换柱净化,正己烷液液分离,硅酸镁固相萃取柱净化,采用UPLC-MS/MS选择离子监测(selected ion monitoring,SIR)正离子模式测定,可对罗非鱼肌肉中甲基睾丸酮残留进行定性和定量检测,检出限为0.4μg/kg,定量限为1μg/kg。线性范围为1～60μg/kg(r>0.999),方法的平均回收率范围为71.06%～83.06%,相对标准偏差为7.4%～15.3%。完全满足食品安全及进出口罗非鱼肌肉中甲基睾丸酮残留的监控和检测需要。
文摘The use of synthetic anabolic steroid methyltestosterone (MT) as growth promoter is prohibited in China. Vali-dations of analytical methods for MT residue in food and the results obtained have become indispensable. The high perfor-mance liquid chromatography (HPLC) method for the detection of MT with liquid-liquid extraction by trichloromethane-methanol in carp muscle tissue was preliminarily validated with reference to the following parameters: recovery (accuracy)at the 1, 5 and 10mg kg-1 level, between-run and within-run CV values (repeatability, also called relative standard deviation(RSD)) and limit of detection. The recoveries were above 80% and the between-run and within-run CV values below 10%for muscle tissue. The limit of detection was 0.05 mg kg-1.
