加速溶剂萃取/气相色谱质谱法测定鱼类样品中的多环麝香  

DETERMINATION OF POLYCYCLIC MUSKS IN FISH SAMPLES BY ACCELERATED SOVENT EXTRACTION(ASE) AND 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》2011年第1期362-365,共4页Environmental Chemistry

基　　金：国家自然科学基金项目(No.20837003;20921063;20890111);国家973项目子课题(No.2009CB421605)资助

摘　　要：建立了鱼类样品中5种多环麝香的分析方法.采用加速溶剂萃取(ASE)提取,经凝胶渗透色谱(GPC)以及中性氧化铝层析柱净化后,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92.7%—112.9%.以六氯苯(13C)为内标,5种合成麝香的线性范围为1.0—1000.0 n.gg-1.麝香的检出限为0.20—0.30 n.gg-1(S/N=3).5种化合物的基质加标回收实验的平均回收率为89.6%—110.1%,RSD为3.2%—8.8%.方法准确,可用于实际样品的检测.An accelerated solvent extraction（ASE） method has been developed to determine five polycyclic musk fragrances in fish samples by GC-MS.Fish samples were extracted by n-hexane,cleaned up by gel permeation chromatography（GPC） and activated neutral Al2O3 column.The final elute was concentrated with nitrogen before injection.Identification was carried out by GC-MS selective ion monitor（SIM） mode.The recovery of fluenthene-d10,surrogate standard,was from 92.7% to 112.9%.The limits of detection were from 0.20 to 0.30 ng·g-1（S/N=3）.Using hexachlorobenzene（HCB） 13C6 as the internal standard,the calibration curves were linear between the concentrations from 1.0 to 1000.0 ng·g-1.The accuracy of the method was evaluated by recovery measurements on spiked samples,and good recoveries（89.6%—110.1%） with low relative standard deviations from 3.2% to 8.8% were achieved when spiked with 100 μg·L-1 standards.The method is accurate during the inspection of synthetic musks in fish samples.

关 键 词：加速溶剂萃取(ASE) 凝胶渗透色谱(GPC) 多环麝香 鱼类样品 GC-MS 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]