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.