凝胶色谱净化-气相色谱-质谱法同时测定烧烤肉制品中19种多环芳烃

Simultaneous Determination of 19 Polycyclic Aromatic Hydrocarbons in Barbecue Meat by GC-MS with Purification by GPC

提出了凝胶色谱净化-气相色谱-质谱法同时测定烧烤肉中19种多环芳烃含量的方法.烧烤肉样品经正己烷-二氯甲烷(1+1)溶液超声提取30 min后,上清液经凝胶色谱净化,所得净化液用HP-5MS色谱柱分离,全扫描模式和选择离子监测模式测定.19种多环芳烃的峰面积与质量浓度在5～200 μg·L-1范围内呈线性关系,检出限(3S/N)在0.1～0.5μg·kg-1之间.在20,40,80 μg·kg-13个浓度水平进行加标回收试验,19种多环芳烃的回收率在58.0％～122％之间,相对标准偏差(n=6)小于21.5％.

A method of GCMS with purification by gel permeation chromatography (GPC) for the simultaneous determination of 19 polycyclic aromatic hydrocarbons (PAH's) in barbecue meat was proposed.The sample was extracted ultrasonically with mixture of n-hexane-dichloromethane (1+ 1) for 30 min,and the extract was purified by gel permeation chromatography.HP-5MS column was used for GC separation,and full-scanning mode as well as selected ion monitoring mode was adopted in MS determination.Linear relationships between values of peak area and mass concentration of the 19 PAH's were kept in the same range of 5-200 μg · L-1,with detection limits (3S/N) in the range of 0.1-0.5 μg · kg-1.Tests for recovery were made at 3 concentration levels of 20,40 and 80 μg · kg-1 of the mixed standards,values of recovery found were in the range of 58.0％-122％ with RSD's (n-6) less than 21.5％.