现代食品科技2018，Vol.34Issue(4)：281-286,214,7.DOI:10.13982/j.mfst.1673-9078.2018.04.041
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
Detection of Six Steroid Hormone Residues in Butter Samples by Gel Permeation Chromatography Purification and Gas Chromatography-Mass Spectrometry
摘要
Abstract
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.关键词
激素/黄油/凝胶渗透色谱/气相色谱-质谱Key words
hormones/butter/gel permeation chromatography/gas chromatography-mass spectrometry引用本文复制引用
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):281-286,214,7.基金项目
上海出入境检验检疫局科技项目(HK004-2016) （HK004-2016）
上海市科委科研项目(16142201500、15395810100、17DZ2293700、17DZ2201100) （16142201500、15395810100、17DZ2293700、17DZ2201100）
长三角科技合作项目(17395810102) （17395810102）
中央引导地方科技发展专项(YDZX20173100004528) （YDZX20173100004528）
