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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
引用本文: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. DOI: 10.7506/spkx1002-6630-201122051
作者姓名:祝璟琳  杨弘  肖炜  邹芝英  李大宇  单航宇
作者单位: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
基金项目: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)
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 chromatography-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。

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  

Determination of Methyltestosterone Residue in Tilapia Muscle by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry(UPLC-MS/MS)
ZHU Jing-lin,YANG Hong,XIAO Wei,ZOU Zhi-ying,LI Da-yu,SHAN Hang-yu. Determination of Methyltestosterone Residue in Tilapia Muscle by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry(UPLC-MS/MS)[J]. Food Science, 2011, 32(22): 243-247. DOI: 10.7506/spkx1002-6630-201122051
Authors:ZHU Jing-lin  YANG Hong  XIAO Wei  ZOU Zhi-ying  LI Da-yu  SHAN Hang-yu
Affiliation:(Key Laboratory of Freshwater Fisheries and Germplasm Resources Utilization, Ministry of Agriculture, Freshwater Fisheries ResearchCenter, Chinese Academy of Fishery Sciences, Wuxi 214081, China)
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 ext...
Keywords:ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  methyltestosterone  tilapia muscle  
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