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凝胶渗透色谱净化-气相色谱-质谱法测定黄油中6种激素的残留
引用本文:赵超敏,古淑青,郑江,邓晓军,岳振峰,赖富饶,闵甜,刘绍杰.凝胶渗透色谱净化-气相色谱-质谱法测定黄油中6种激素的残留[J].现代食品科技,2018,34(4):281-286.
作者姓名:赵超敏  古淑青  郑江  邓晓军  岳振峰  赖富饶  闵甜  刘绍杰
作者单位:上海出入境检验检疫局动植物与食品检验检疫技术中心;深圳出入境检验检疫局食品检验检疫技术中心;华南理工大学食品科学与工程学院;山东省莘县农业局
基金项目:上海出入境检验检疫局科技项目(HK004-2016);上海市科委科研项目(16142201500、15395810100、17DZ2293700、17DZ2201100);长三角科技合作项目(17395810102);中央引导地方科技发展专项(YDZX20173100004528)
摘    要:建立了凝胶渗透色谱(GPC)-气相色谱-质谱(GC/MS)同时测定黄油中雄酮(A)、脱氢表雄酮(DHEA)、睾酮(T)、孕酮(P)、雌酮(E1)、17β-雌二醇(β-E)6种类固醇激素残留的方法。黄油样品用乙酸乙酯/环己烷(1:1,V/V)振荡辅助提取,提取液经GPC柱净化除脂,GPC浓缩液用氮气吹至尽干,然后用乙酸酐和吡啶衍生化,最后,衍生化物经GC色谱柱(HP-5MS,30 m×0.25mm,0.25μm)分离,在SIM模式下进行定性和定量分析。6种类固醇激素以外标法定量,在10~500μg/kg线性范围内相关系数(r)均大于0.999;方法的定量限LOQs(S/N≥10)为4~10μg/kg;添加水平为10μg/kg、50μg/kg、200μg/kg时,加标回收率范围为77.2~112%,相对标准偏差为4.2~10%。结果表明,所建方法准确、可靠,已成功用于黄油中6种类固醇激素的检测分析。

关 键 词:激素  黄油  凝胶渗透色谱  气相色谱-质谱
收稿时间:2017/10/20 0:00:00

Detection of Six Steroid Hormone Residues in Butter Samples by Gel Permeation Chromatography Purification and Gas Chromatography-Mass Spectrometry
ZHAO Chao-min,GU Shu-qing,ZHENG Jiang,DENG Xiao-jun,YUE Zhen-feng,LAI Fu-rao,MIN Tian and LIU Shao-jie.Detection of Six Steroid Hormone Residues in Butter Samples by Gel Permeation Chromatography Purification and Gas Chromatography-Mass Spectrometry[J].Modern Food Science & Technology,2018,34(4):281-286.
Authors:ZHAO Chao-min  GU Shu-qing  ZHENG Jiang  DENG Xiao-jun  YUE Zhen-feng  LAI Fu-rao  MIN Tian and LIU Shao-jie
Affiliation:(1.Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China),(1.Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China),(1.Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China),(1.Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China),(2.Food Inspection Center, Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518045, China),(3.School of Food Sciences and Engineering, South China University of Technology, Guangzhou 510640, China),(3.School of Food Sciences and Engineering, South China University of Technology, Guangzhou 510640, China) and (4.Shandong Shen County Agriculture Bureau, Liaocheng 252400, China)
Abstract:
Keywords:hormones  butter  gel permeation chromatography  gas chromatography-mass spectrometry
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