气相色谱-质谱联用法测定橡胶胶塞中的15种多环芳烃

Determination of 15 plugpolycyclic aromatic hydrocarbons in the rubber plug by gas chromatography and mass spectrometry

目的建立气相色谱-质谱联用法测定橡胶胶塞中15种多环芳烃(PAHs)的含量。方法甲苯加热方法提取橡胶塞中的PAHs。采用多环芳烃专用气相毛细管Agilent DB-EUPAH(20 m×0.18 mm),程序升温的气相方法,选择离子模式采集数据。同时测定线性范围、检出限、定量限、精密度、重复性和回收率。结果 15种PAHs在相应浓度范围内线性关系良好,相关系数(r)均>0.999,检出限为0.512 ng/ml^9.910 ng/ml,定量限为1.705 ng/ml^33.034 ng/ml,精密度实验RSD<4.0%,重复性实验RSD<3.0%,平均加样回收率为91.0%~93.7%。结论本研究建立的气相-质谱联用测定15种PAHs方法良好,选择性和灵敏度高,橡胶胶塞样品提取液中的复杂基质物质对本方法检测干扰小,该方法能够快捷、简便、准确的检测出橡胶胶塞中15种PAHs的含量,适用于橡胶胶塞中PAHs的测定。

Objective To establish a gas chromatography and mass spectrometry（ GC- MS） method for the determination of 15 plugpolycyclic aromatic hydrocarbons（ PAHs） in rubber plug. Methods Extract the PAHs from the rubber plug through toluene heating. Analysis was carried on an Agilent DB- EUPAH（ 20 m × 0. 18 mm） column special for polycyclic aromatic hydrocarbons,with temperature programming in data acquisition mode of SIM. To test linearity,LOD,LQD,precision,repeatability and recovery. Results A good linear relationship was obtained when the concentrations of the 15 PAHs were within the certain ranges,with the correlative coefficient（ r）〉 0. 999; LOD was within 0. 512 ng / ml- 9. 910 ng / ml; LQD was with 1. 705 ng / ml-33. 034 ng / ml; RSD of precision test was less than 4. 0 %,repeatability RSD was less than 3. 0 %; the average recovery rate was within 91. 0 %- 93. 7 %. Conclusion In this study,15 PAHs methods established for the determination is good,high selective and high sensitive. Interference of the complex material is small for the detection. So the method is rapid,simple,accurate and reliable for the determination of PAHs in the rubber plug.