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。
A gel permeation chromatography purification（GPC）-gas chromatography-mass spectrometry（GC/MS） method was developed for the determination of 6 steroid hormone residues（androsterone（A）, dehydroepiandrosterone（DHEA）, testosterone（T）, progesterone（P）, estrone（E1） and β-estradiol（β-E）） in butter samples. The butter samples were extracted by oscillation with ethylacetate/cyclohexane（1：1, V/V）. The extract was purified and degreased by GPC column. The GPC concentrate was evaporated to dryness under a stream of nitrogen. Derivatization of the residue was carried out with pyridine and aceticanhydride. Finally, the derivative was separated using a GC column（HP-5 MS, 30 m×0.25 mm, 0.25 μm）, and the qualitative and quantitative analysis was conducted under the model of selective ion monitor（SIM）. Steroid hormone residues were quantified using external standard method, which had good linearity in the concentration range of 10-500 μg/kg with correlation coefficiency larger than 0.999. The quantification limit was 4-10 μg/kg. At the spike levels of 10 μg/kg, 50 μg/kg and 200 μg/kg, the recoveries of hormones were in the range of 77.2-112% and the relative standard deviation（RSD） was from 4.2% to 10%. The above results showed that the method was accurate, reliable and suitable for the determination of 6 hormone residues in butter samples.
作者
赵超敏
古淑青
郑江
邓晓军
岳振峰
赖富饶
闵甜
刘绍杰
ZHAO Chao-min1, GU Shu-qing1, ZHENG Jiang1, DENG Xiao-jun1, YUE Zhen-feng2, LAI Fu-rao3, MIN Tian3, LIU Shao-jie4(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;4.Shandong Shen Cotmty Agriculture Bureau, Liaocheng 252400, Chin)
出处
《现代食品科技》
EI
CAS
北大核心
2018年第4期281-286,214,共7页
Modern Food Science and Technology
基金
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)
关键词
激素
黄油
凝胶渗透色谱
气相色谱-质谱
hormones
butter
gel permeation chromatography
gas chromatography-mass spectrometry
