食品科学2011,Vol.32Issue(22):243-247,5.
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
Determination of Methyltestosterone Residue in Tilapia Muscle by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry(UPLC-MS/MS)
摘要
Abstract
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.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Key words
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)/methyltestosterone/tilapia muscle分类
轻工纺织引用本文复制引用
祝璟琳,杨弘,肖炜,邹芝英,李大宇,单航宇..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[J].食品科学,2011,32(22):243-247,5.基金项目
现代农业产业技术体系建设专项 ()
2007年公益性行业(农业)科研专项 ()
中央级公益性科研院所基本科研业务费专项 ()