| 气相色谱/燃烧炉/同位素比质谱法溯源分析黄油中5种类固醇激素 |
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| 引用本文： | 赵超敏,古淑青,曲栗,韩丽,肖陈贵,邓晓军,岳振峰,王传现,房克艳. 气相色谱/燃烧炉/同位素比质谱法溯源分析黄油中5种类固醇激素[J]. 现代食品科技, 2019, 35(2): 270-278 |
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| 作者姓名： | 赵超敏 古淑青 曲栗 韩丽 肖陈贵 邓晓军 岳振峰 王传现 房克艳 |
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| 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,上海,200135;深圳出入境检验检疫局食品检验检疫技术中心,广东深圳,518045;上海出入境检验检疫局动植物与食品检验检疫技术中心,上海200135;上海大学生命科学学院,上海200444 |
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| 基金项目： | 上海市科委科研项目（16142201500；17DZ2293700；18DZ2201200；17DZ2201100）；长三角科技合作项目（17395810102）；中央引导地方科技发展专项（YDZX20173100004528） |
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| 摘 要： | 建立了黄油中雌酮、α/β-雌二醇、雌三醇和孕酮5种类固醇激素的气相色谱/燃烧炉/同位素比质谱(GC/C/IRMS)溯源方法。样品经乙酸乙酯-环己烷(1:1,V/V)提取,经凝胶渗透色谱(GPC)净化和半制备液相色谱(Pre-HPLC)纯化,纯化液经HP-5MS(30 m×0.25 mm,0.25μm)柱分离,GC/C/IRMS溯源分析和气相色谱-质谱(GC/MS)定性和定量分析。黄油中外源性激素δ~(13)C值-30‰,内源性激素δ~(13)C值-27‰,其中黄油中外源性孕酮δ~(13)C值=-30.59‰±0.12‰,内源性孕酮δ~(13)C值范围在-26.83‰±0.25‰与-23.80‰±0.33‰之间,单因素方差分析(p值=0.0090.05)显示内源性孕酮和外源性孕酮的δ~(13)C值存在显著差异性。经模拟实验显示,实际样品中引入外源性激素的δ~(13)C值与外源性激素δ~(13)C值具有同源性。方法灵敏度为15～100ng,方法批内精密度为0.11‰～0.17‰,批间精密度为0.16‰,Pre-HPLC的馏分接收是同位素分馏现象发生和影响测定准确性的主要阶段。结果表明,本方法准确性和特异性好,GC/C/IRMS是鉴别激素来源的有效工具。
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| 关 键 词： | 内源性激素 外源性激素 黄油 气相色谱/燃烧炉/同位素比质谱 溯源 |
| 收稿时间： | 2018-08-28 |
Traceability of Five Steroid Hormones in Butter Investigated by Gas Chromatography-combustion-isotope Ratio Mass Spectrometry |
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| ZHAO Chao-min,GU Shu-qing,QU Li,HAN Li,XIAO Chen-gui,DENG Xiao-jun,YUE Zhen-feng,WANG Chuan-xian and FANG Ke-yan. Traceability of Five Steroid Hormones in Butter Investigated by Gas Chromatography-combustion-isotope Ratio Mass Spectrometry[J]. Modern Food Science & Technology, 2019, 35(2): 270-278 |
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| Authors: | ZHAO Chao-min GU Shu-qing QU Li HAN Li XIAO Chen-gui DENG Xiao-jun YUE Zhen-feng WANG Chuan-xian FANG Ke-yan |
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| 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),(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),(1.Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China) and (1.Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China)(3.School of Life Sciences, Shanghai University, Shanghai 200444, China) |
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| Abstract: | |
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| Keywords: | endogenous hormone exogenous hormone butter gas chromatography/combustion/isotope ratio mass spectrometry traceability |
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