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气相色谱-质谱法测定人体血液样品中合成麝香

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胡正君, 史亚利, 蔡亚岐. 气相色谱-质谱法测定人体血液样品中合成麝香[J]. 环境化学, 2010, 29(3): 530-535.
引用本文: 胡正君, 史亚利, 蔡亚岐. 气相色谱-质谱法测定人体血液样品中合成麝香[J]. 环境化学, 2010, 29(3): 530-535.
shu
HU Zheng-jun, SHI Ya-li, CAI Ya-qi. DETERMINATION OF SYNTHETIC MUSKS IN HUMAN BLOOD BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY[J]. Environmental Chemistry, 2010, 29(3): 530-535.
Citation: HU Zheng-jun, SHI Ya-li, CAI Ya-qi. DETERMINATION OF SYNTHETIC MUSKS IN HUMAN BLOOD BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY[J]. Environmental Chemistry, 2010, 29(3): 530-535.
shu

气相色谱-质谱法测定人体血液样品中合成麝香

  • 1.

    中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室, 北京, 100085

  • 基金项目:

    国家自然科学基金重点项目(No.20837003)

    国家自然科学基金创新群体(20921063)资助项目

DETERMINATION OF SYNTHETIC MUSKS IN HUMAN BLOOD BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY

  • 1.

    State Key Laboratory of Environmental Chemistry and Ecotoxicity, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing, 100085, China

  • Fund Project:

  • 摘要: 采用气相色谱-质谱联用技术(GC-MS),建立了测定人全血样品中5种多环麝香和2种硝基麝香的分析方法.血液样品前处理采用正己烷液-液萃取,硅胶柱层析净化,洗脱液经N2浓缩后用GC-MS选择离子监测模式(SIM)进行检测.使用该前处理方法,替代物标样荧蒽-d10的回收率为85%—120%.以六氯苯(13C)为内标进行定量,7种合成麝香的线性范围为0.5—10μg·l-1,检出限在0.25—0.30μg·l-1(S/N=3)范围内.应用本方法,对实际全血样品进行3个不同浓度的加标回收实验,所得合成麝香的平均加标回收率均在77.9%—118.5%范围内,相对标准偏差在1.5%—9.5%之间.
    Abstract: A novel method has been developed to determine five polycyclic musk fragrances and two nitro musk fragrances in human blood by GC-MS.Blood samples were extracted by n-hexane,cleaned up by silica gel column,and final eluate was concentrated with nitrogen before injection.Identification was carried out by GC-MS in the Selective Ion Monitor(SIM)mode.The recovery of fluenthene-d10,surrogate standard,was from 85.0% to 120.0%.The detection limits were from 0.25 to 0.30 μg·l-1(S/N=3).Using hexachlorobenzene(HCB)13C6 as the internal standard,good linear calibrations were obtained over the range of 0.5 to 10μg·l-1.Under the optimum conditions,the synthetic musk fragrances were recovered well at three different spiked concentrations with the recoveries ranging from 77.9% to 118.5%,and relative standard deviations ranging from 1.5% to 9.5%.
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  • 收稿日期:  2009-05-20
胡正君, 史亚利, 蔡亚岐. 气相色谱-质谱法测定人体血液样品中合成麝香[J]. 环境化学, 2010, 29(3): 530-535.
引用本文: 胡正君, 史亚利, 蔡亚岐. 气相色谱-质谱法测定人体血液样品中合成麝香[J]. 环境化学, 2010, 29(3): 530-535.
shu
HU Zheng-jun, SHI Ya-li, CAI Ya-qi. DETERMINATION OF SYNTHETIC MUSKS IN HUMAN BLOOD BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY[J]. Environmental Chemistry, 2010, 29(3): 530-535.
Citation: HU Zheng-jun, SHI Ya-li, CAI Ya-qi. DETERMINATION OF SYNTHETIC MUSKS IN HUMAN BLOOD BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY[J]. Environmental Chemistry, 2010, 29(3): 530-535.
shu

气相色谱-质谱法测定人体血液样品中合成麝香

  • 1. 中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室, 北京, 100085
  • 收稿日期:  2009-05-20
基金项目:

国家自然科学基金重点项目(No.20837003)

国家自然科学基金创新群体(20921063)资助项目

摘要: 采用气相色谱-质谱联用技术(GC-MS),建立了测定人全血样品中5种多环麝香和2种硝基麝香的分析方法.血液样品前处理采用正己烷液-液萃取,硅胶柱层析净化,洗脱液经N2浓缩后用GC-MS选择离子监测模式(SIM)进行检测.使用该前处理方法,替代物标样荧蒽-d10的回收率为85%—120%.以六氯苯(13C)为内标进行定量,7种合成麝香的线性范围为0.5—10μg·l-1,检出限在0.25—0.30μg·l-1(S/N=3)范围内.应用本方法,对实际全血样品进行3个不同浓度的加标回收实验,所得合成麝香的平均加标回收率均在77.9%—118.5%范围内,相对标准偏差在1.5%—9.5%之间.

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