摘要：本文建立了一种加速溶剂萃取-固相萃取净化-气相色谱/质谱联用（ASE-SPE-GC-MS）方法，用于同步测定土壤中有机氯农药与多氯联苯。以二氯甲烷-正己烷（体积比1:1）为提取溶剂，经2次萃取后，采用氮吹浓缩至约1mL；随后通过固相萃取小柱（SPE）净化，并用正己烷-二氯甲烷（体积比9:1）洗脱，收集洗脱液再次氮吹浓缩至1mL，过 0.45μm滤膜后进行GC-MS定量分析。21种有机氯农药和15种多氯联苯的校准曲线中目标化合物相对响应因子的相对标准偏差均小于30%，在2.5μg/kg、25μg/kg两个加标水平下36种SVOCs的加标回收率为44%～103%，检出限为0.27μg/kg~1.42μg/kg，测定下限为1.08μg/kg~5.68μg/kg。
关键词：土壤；有机氯；多氯联苯；加速溶剂萃取；气相色谱-质谱法
Abstract: This article establishes an accelerated solvent extraction solid phase extraction purification gas chromatography/mass spectrometry (ASE-SPE-GC-MS) method for simultaneous determination of organochlorine pesticides and polychlorinated biphenyls in soil. Using dichloromethane and n-hexane (volume ratio 1:1) as the extraction solvent, after two extractions, the extrac was concentrated to about 1mL by nitrogen blowing. Then, it was purified by solid-phase extraction column (SPE) and eluted with n-hexane dichloromethane (volume ratio 9:1). The eluent was collected and concentrated again by nitrogen blowing to 1mL. After passing through a 0.45 μ m filter membrane, it was quantitatively analyzed by GC-MS. The relative standard deviations of the response factors of target compounds in the calibration curves of 21 organochlorine pesticides and 15 polychlorinated biphenyls are all less than 30%. The spiked recovery rates of 36 SVOCs at two spiked levels of 2.5 μ g/kg and 25 μ g/kg are 44%~103%, with a detection limit of 0.27 μ g/kg~1.42 μ g/kg and a lower limit of determination of 1.08 μ g/kg~5.68 μ g/kg.
Keywords：soil；polychlorinated biphenyls；organochlorine pesticides；Accelerated solvent extraction；gas chromatography-mass spectrometry （GC-MS）
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