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采用自动固相萃取-气相色谱/质谱技术,建立了地表水中痕量多环芳烃和有机氯农药的检测方法。调节水样pH<2,加入1%甲醇,使用C18固相萃取柱富集,3 mL丙酮+3 mL二氯甲烷洗脱后浓缩定容。采用气相色谱/质谱联用的全扫描模式进行分析,选择特征离子定量,方法检出限为0.026~8.772 ng/L。加标水平为0.1μg/L时,样品加标回收率在74.8%~109%之间,RSD为0.01%~14.5%。该方法自动化程度高、快速、准确、重复性好,能满足地表水体中持久性有机污染物分析的要求。
The detection methods of trace polycyclic aromatic hydrocarbons (PAHs) and organochlorine pesticides (PAHs) in surface water were established by automatic solid phase extraction coupled with gas chromatography / mass spectrometry. Adjust the water sample pH <2, add 1% methanol, enrich with C18 solid phase extraction column, elute with 3 mL acetone + 3 mL dichloromethane, and concentrate and dilute to volume. The full-scan mode of GC / MS was used to analyze the characteristic ions. The detection limits were 0.026-8.772 ng / L. The spiked recoveries of spiked samples ranged from 74.8% to 109% at spiking levels of 0.1 μg / L with RSD of 0.01% to 14.5%. The method is highly automated, fast, accurate and reproducible, and can meet the requirements of POPs analysis in surface water.