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目的建立全自动固相萃取-气相色谱/质谱联用法快速检测饮用水源中16种多环芳烃,了解本市饮用水源中多环芳烃的污染状况。方法水样用盐酸调p H<2,再加入30ml甲醇混匀上样,上样流速为10 ml/min,被测物质经Thermo Hyper Sep C18小柱富集后,用乙酸乙酯和二氯甲烷洗脱,采用程序升温,TG-5MS色谱柱分离,质谱检测,利用保留时间和选择离子监测(SIM)模式进行定性定量。结果 16种化合物相关系数大于0.998,检出限(MDL)为0.0069ng/L~0.074ng/L,样品平均加标回收率在82.5%~119.2%之间,相对标准偏差(RSD)6.07%~9.97%。结论该方法具有较高的准确度与精密度,操作简便、快速,溶剂用量少,适合于水中16种多环芳烃的测定。
OBJECTIVE To establish an automatic SPE-GC / MS method for the rapid determination of 16 PAHs in drinking water and to understand the status of polycyclic aromatic hydrocarbons (PAHs) in drinking water sources in this Municipality. Methods The samples were adjusted to pH pH <2 with hydrochloric acid, and then added with 30 ml of methanol. The flow rate of the sample was 10 ml / min. After the sample was concentrated on a Thermo Hyper Sep C18 cartridge, the sample was eluted with ethyl acetate and dichloro Methane elution, temperature programmed, TG-5MS column separation, mass spectrometry detection, the use of retention time and selected ion monitoring (SIM) mode for qualitative and quantitative. Results The correlation coefficient of 16 compounds was more than 0.998, the detection limit (MDL) was 0.0069ng / L ~ 0.074ng / L, the average recoveries were between 82.5% and 119.2%, and the relative standard deviations (RSDs) were 6.07% 9.97%. Conclusion The method has high accuracy and precision, easy to operate, fast, less solvent and suitable for the determination of 16 PAHs in water.