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。
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.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2011年第22期243-247,共5页
Food Science
基金
现代农业产业技术体系建设专项(CARS-49)
2007年公益性行业(农业)科研专项(3-49)
中央级公益性科研院所基本科研业务费专项(2009JBFB04)
作者简介
祝璟琳（1983--），男，助理研究员，硕士，研究方向为食品安全和水产病害。E—mail：zhujl@ffrc．cn
通信作者：杨弘（1966-），男，研究员，本科，研究方向为生物技术和鱼类遗传育种。E-mail：yangh@ffrc．cn
