加速溶剂萃取气相色谱质谱法测定污泥、底泥及土壤样品中的合成麝香  

Determination of Synthetic Musk Fragrances in Sewage Sludge,Sediment and Soil Using Accelerated Solvent Extraction 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：《分析化学》2010年第6期885-888,共4页Chinese Journal of Analytical 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(No.20921063);国家973项目子课题(No.2009CB421605)资助

摘　　要：建立了污泥、底泥及土壤样品中7种合成麝香的分析方法。采用加速溶剂萃取(ASE)提取,经硅胶/中性氧化铝复合层析柱净化后,浓缩并定容洗脱液,用GC-SIM-MS进行检测。本方法对替代物标样荧蒽-d10的回收率为89.7%～110.9%。以六氯苯-c13为内标,7种合成麝香的线性范围为0.6～100.0μg/kg。底泥和土壤中麝香的检出限为0.25～0.33μg/kg(S/N=3);污泥中的检出限为2.9～3.3μg/kg(S/N=3)。基质加标回收实验的平均回收率为83.6%～105.1%;RSD为3.2%～9.8%。本方法准确、快速,可用于实际样品的检测。A rapid, simple accelerated solvent extraction （ASE） method has been developed to determine seven synthetic musks in sewage sludge, sediment and soil by GC-MS. After extraction, samples were cleaned up by silica gel/ neutral Al2O3column. Then final eluate was concentrated before injection. Identification was carried out by GC-MS in the Selective Ion Monitor （SIM） mode. Using the method, the recovery of fluenthene-d10, surrogate standard, was from 89.7% to 110.9%. The detection limits of musks were from 2.9 to 3.3 μg/kg in sewage sludge and 0.25-0.33 μg/kg in sediment and soil（S/N=3）. Using hexachlorobenzene （HCB） 13C6 as the internal standard, good linear calibrations were obtained in the range of 0.6-100 μg/kg. The average recoveries were in the range of 83.6%-105.1% when the spiked concentration was 10 μg/kg. The RSD ranged from 3.2% to 9.8%. The method is accurate during the inspection of synthetic musks in real samples.

关 键 词：加速溶剂萃取 合成麝香 污泥 底泥 土壤 硅胶/中性氧化铝复合层析柱 气相色谱-质谱联用 

分 类 号：X833[环境科学与工程—环境工程]