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采用自动索氏抽提-凝胶渗透色谱(GPC)-气相色谱/质谱技术,建立了沉积物中多环芳烃和有机氯农药的检测方法.通过对自动索氏抽提提取条件、凝胶渗透色谱净化条件进行优化.以丙酮∶正己烷(V∶V=1∶1)作为提取溶剂,提取温度160℃,用乙酸乙酯∶环己烷(V∶V=1∶1)定容至40 mL,转移上GPC.GPC在线浓缩系统真空腔真空度为180 mbar/190 mbar,以乙酸乙酯∶环己烷(V∶V=1∶1)为流动相,流速为5 mL·min-1,并采用气相色谱-质谱法定性和定量分析.在优化条件下,16种多环芳烃和19种有机氯农药在10—1000μg·L-1范围内具有良好的线性关系(R2>0.99),检出限(S/N=3)为0.008—0.353μg·kg-1.加标水平为10、50、100μg·kg-1时,平均加标回收率分别为77.6%—106.1%、79.9%—108.7%和80.6%—107.8%,相对标准偏差(RSDs,n=5)均小于10%.
The detection method of polycyclic aromatic hydrocarbons and organochlorine pesticides in sediments was established by automatic Soxhlet extraction-gel permeation chromatography (GPC) -gas chromatography / mass spectrometry.By analyzing the extraction conditions of automatic Soxhlet extraction, gel permeation Chromatographic purification conditions were optimized.The extraction temperature was 160 ℃ with acetone: n-hexane (V: V = 1: 1) as the extraction solvent and the volume was fixed to 40 with ethyl acetate: cyclohexane mL and transferred to GPC.GV vacuum concentration of GPC online concentration system was 180 mbar / 190 mbar, the mobile phase was ethyl acetate: cyclohexane (V:V = 1: 1), the flow rate was 5 mL · min -1 , And analyzed by gas chromatography-mass spectrometry (GC-MS) qualitatively and quantitatively.Under the optimal conditions, 16 PAHs and 19 organochlorine pesticides had a good linear relationship (R2> 0.99) in the range of 10-1000μg · L-1, The detection limit (S / N = 3) was 0.008-0.353μg · kg-1, and the average recoveries were 77.6% -106.1% and 79.9% at the spiked levels of 10, 50 and 100μg · kg- -108.7% and 80.6% -107.8% respectively. The relative standard deviations (RSDs, n = 5) were less than 10%.