环境水样中人工合成麝香的分析方法  

DETERMINATION OF SYNTHETIC MUSK FRAGRANCES IN ENVIRONMENTAL WATER SAMPLES WITH 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6期1172-1176,共5页Environmental Chemistry

基　　金：国家自然科学基金重点项目(No.20837003);国家自然科学基金重大项目(20897010);国家973项目子课题(2009CB421605)资助

摘　　要：采用C18萃取盘富集净化结合气相色谱-质谱联用技术(GC-MS),建立了测定城市污水和河水中5种多环麝香和2种硝基麝香的分析方法.水样经C18萃取盘富集后,用正己烷及正己烷、二氯甲烷混合溶剂进行洗脱,洗脱液经浓缩定容后用GC-MS选择离子监测模式(SIM)进行检测,使用AHTN-d3作为替代物标样,其回收率为89.7%—104.9%.以六氯苯-13C为内标进行定量,7种合成麝香的线性范围为0.001—1μg·ml-1,样品方法检出限在1.0—1.2ng·l-1(S/N=5).做空白加标实验和基质加标回收实验,空白加标回收率及实际样品平均加标回收率均在78.6%—106.3%范围内,相对标准偏差在3.9%—8.4%之间;方法准确,快速,简便,可以用于实际水样中合成麝香的检测。A method has been developed to determine five polycyclic musk fragrances and two nitro musk fragrances in environmental water samples from wastewater treatment plants and river by GC-MS.Samples were concentrated by C18 discs and eluted by hexane or a mixture of hexane and methylene chloride.Identification was carried out by GC-MS in the Selective Ion Monitor（SIM） mode.The recovery of AHTN-d3,surrogate standard,was from 89.7% to 104.9%.Using hexachlorobenzene（HCB） 13C6 as the internal standard,good linear calibrations were obtained over the range of 0.001 to 1μg·ml-1.The detection limits were from 1 to 1.2 ng·l-1 in water samples（S/N = 5）.Under spiked conditions,the synthetic musk fragrances were recovered well,with the recoveries ranging from 78.6% to 106.3% in water samples.Moreover,the relative standard deviations were from 3.9% to 8.4%.The method is accurate,rapid and suitable for the inspection of synthetic musk fragrances in real samples.

关 键 词：C18萃取盘 合成麝香 环境水样 GC-MS 

分 类 号：X832[环境科学与工程—环境工程]