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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

祝璟琳 杨弘 肖炜 邹芝英 李大宇 单航宇

食品科学2011,Vol.32Issue(22):243-247,5.
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)

祝璟琳 1杨弘 1肖炜 1邹芝英 1李大宇 1单航宇1

作者信息

  • 1. 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,江苏无锡214081
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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 ()

食品科学

OA北大核心CSCDCSTPCD

1002-6630

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