气相色谱-质谱法测定人体血液样品中合成麝香  

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

作　　者：胡正君[1] 史亚利[1] 蔡亚岐[1] 

机构地区：[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

出　　处：《环境化学》2010年第3期530-535,共6页Environmental Chemistry

基　　金：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.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）13C6as 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%.

关 键 词：合成麝香 人体全血 气相色谱-串联质谱(GC-MS) 

分 类 号：R115[医药卫生—公共卫生与预防医学]