气相色谱-质谱联用法测定水产品中16种多环芳烃

Determination of 16 polycyclic aromatic hydrocarbons in aquatic products by GC/MS

目的：建立水产品中16种多环芳烃的测定方法。方法：试样用氢氧化钾-甲醇溶液皂化,环己烷萃取,甲醇溶液清洗,硫酸溶液处理,硅胶柱净化,用气相色谱-质谱联用仪测定,内标法定量。结果：检测的16种多环芳烃中,萘、苊烯、苊、芴、菲、蒽、芘、苯并[a]蒽在0.05-10.0μg/ml浓度范围,其余化合物在0.1-10μg/ml浓度范围,呈良好的线性相关,相关系数r＆gt;0.998;以2、20、100μg/kg 3个水平进行加标回收实验,16种多环芳烃的回收率为60.2%-103.8%,RSD〈15%;当加标量为2μg/kg时16种多环芳烃均具有明显的峰形,响应值最低的二苯并[a,h]蒽的信噪比≥10。结论：该方法灵敏度和重现性好,是分析水产品是否受环境污染物PAHs污染的理想方法。

Objective：To establish a GC/MS method for determination of 16 polycyclic aromatic hydrocarbons （PAHs） in aquatic products. Methods ：The samples were extracted with cyclohexane after KOH-MeOH saponification and cleaned up by the columns of neutral silica gel. Results：The 16 PAHs had good linearity （r 〉0. 998）, in the range of 0. 05 - 10. 0 μg/ml, the recoveries were 60. 2% - 103.8%, spiked at three different levels. RSD 〈 15% （ n =6） ,and the limit of detection of 16 PAHs was 2 μg/kg. Conclusion ：The method is sensitive, accurate, rapid and of high recovery. It can be used for the quality control of 16 PAHs in aquatic products.