同位素稀释高分辨质谱法测定鱼组织中6种多环芳烃

Determination of Six Polycyclic Aromatic Hydrocarbons in Fish Tissue by Isotope Dilution GC/HRMS

采用气相色谱一双聚焦高分辨磁式质谱联用仪开发了同位素稀释质谱法（IDMS）测定鱼组织中6种多环芳烃（PAHs）。以二氯甲烷为提取溶剂，将冻干鱼组织样品加入氘代的同位素内标后，在50℃下索氏提取18h，采用凝胶排阻色谱（GPC）联用，固相萃取（SPE）进行净化，通过条件优化，采用二氯甲烷作为GPC的流动相，在3．5mL·min^-1流速下，收集14-34min的流出液，浓缩后用氟罗里硅土SPE小柱净化，V（环己烷）：y（二氯甲烷）=1：1的溶液洗脱，以高分辨多离子方法（HRMS-MID）检测，单点校正法定量。6种PAHs在3个添加水平的检测回收率为95％～105％，精密度（RSD）为1．7％～6．0％，最小检出限为0．8～1．6μg·kg^-1。

Abstract：An isotope dilution mass spectrometryt.llJlVlO） meulou t~,l polycyclic aromatic hydrocarbons （PAHs）, including fluoranthene, benzo[b] fluoranthene, benzo[k] fluoranthene, benzo [a]pyrene, benzo [ g, h, i] perylene, indeno [ 1,2,3-c, d]-py- rene, in freezing dried fish tissue was established. 6 PAHs were extracted with dichlo- romethane by soxhlet extraction under 50 ℃ for 18 h. Purification of extracts was carried out by gel permeation chromatography（GPC） and solid phase extraction（SPE）. Dichlo- romethane was chosen as mobile phase after comparing the eluting effect of 6 PAHs with V（ethyl acetate） ： V（cyclohexane） = 1 ： 1, and V（cyclohexane） ： V（dichloromethane） = 1 ： 1 was chosen as eluting solution of SPE after optimizing the type and ratio of eluting so- lution. 6 PAHs were separated by capillary column DB-5（30 m×0.25 mm×0.25 m） with helium as carrying gas. 6 PAHs were quantified by high resolution mass spectrometry multi-ion detection（HRMS-MID）, using deuterated PAHs as internal standards, single point method. The recoveries of 6 PAHs are in the range of 95%-105%. The detection limits of 6 PAHs are 0.8-1.6 μg ·kg-1 （dry weight）. The RSD（n=6） ranges from 1.70/40 to 6. 0%. The methods was applied to three fish sample, the spectrum of the sample showed the little inference and ideal sensitivity of the method. With good sensitivity and accuracy, this method will be successfully applied to the qualitative and quantitative analysis of fish tissue sample.