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当前位置: 首页 > 文章 > 超高效液相色谱-串联质谱联用测定罗非鱼肌肉中甲基睾丸酮残留 食品科学 2011,32 (22) 243-247
Position: Home > Articles > Determination of Methyltestosterone Residue in Tilapia Muscle by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry(UPLC-MS/MS) FOOD SCIENCE 2011,32 (22) 243-247

超高效液相色谱-串联质谱联用测定罗非鱼肌肉中甲基睾丸酮残留

作  者：
祝璟琳;杨弘;肖炜;邹芝英;李大宇;单航宇
单  位：
中国水产科学研究院淡水渔业研究中心农业部淡水渔业和种质资源利用重点实验室
关键词：
超高效液相色谱-串联质谱(UPLC-MS/MS);甲基睾丸酮;罗非鱼肌肉
摘  要：
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。
译  名：
Determination of Methyltestosterone Residue in Tilapia Muscle by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry(UPLC-MS/MS)
作  者：
ZHU Jing-lin,YANG Hong,XIAO Wei,ZOU Zhi-ying,LI Da-yu,SHAN Hang-yu(Key Laboratory of Freshwater Fisheries and Germplasm Resources Utilization,Ministry of Agriculture,Freshwater Fisheries Research Center,Chinese Academy of Fishery Sciences,Wuxi 214081,China)
关键词：
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);methyltestosterone;tilapia muscle
摘  要：
A method for the determination of methyltestosterone in tilapia muscle using ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed.Deuterium-labeled methyltestosterone was used as internal standard and added to the sample before being extracted with acetonitrile.The extract was partitioned into ethyl acetate and cleaned up on a strong anion exchange column.Subsequently,the eluates were further extracted with n-hexane and cleaned up on a magnesium silicate solid phase extraction cartridge before UPLC-MS/MS determination.The mass spectrometer was operated in the positive ion mode using selected ion monitoring for qualitative and quantitative analysis of methyltestosterone.The limit of detection was 0.4 μg/kg and the limit of quantitation was 1μg/kg.The calibration curve was linear with a correlation coefficient of over 0.999 within the concentration range of 1-60μg/kg.The average recoveries for methyltestosterone were 71.06%-83.06% across three spike levels(n=5) with a relative standard deviation(CV) between 7.4% and 15.3%.These results demonstrate that this method fully meets the requirements for the determination of methyltestosterone residue in imported and exported tilapia muscles for the purpose of ensuring food safety.

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