ASE萃取-SPE净化-气相色谱/质谱法同时测定土壤中的16种多环芳烃和8种有机氯农药

Simultaneous Determination of 16 Polycyclic Aromatic Hydrocarbons and 8 Organochlorine Pesticides in Soil Samples by Gas Chromatography/Mass Spectrometry with Accelerated Solvent Extraction Coupled with Solid-phase Extraction Cleanup

建立了加速溶剂萃取-Florisil柱净化-气相色谱/质谱法(GCMS)同时测定新鲜土壤中的16种多环芳烃和8种有机氯农药的分析方法。通过优化GCMS分析参数和ASE条件,用选择离子模式(SIM)检测。结果表明,方法在10～600μg/L范围内线性关系良好,相关系数均大于0.996,各目标化物的方法检出限为0.10～0.31μg/kg,空白硅藻土样品的加标回收率在63.1%～86.7%之间,7次平行测定的相对标准偏差为4.9%～15.1%。用该方法测定云南某地的3个土壤样品,多环芳烃和有机氯农药均有检出,其中多环芳烃质量分数在0.9×10^(-3)～4.7×10^(-3)mg/kg之间,有机氯质量分数在0.8×10^(-3)～6.6×10^(-3)mg/kg之间,适用于土壤样品中多环芳烃和有机氯农药的分析。

This study established a method for determination of 16 kinds of polycyclic aromatic hydrocarbons and8kinds of organochlorine pesticides in soil samples by gas chromatography/mass spectrometry with accelerated solvent extraction.The GCMS analysis parameters and accelerated solvent extraction condition were optimized so that all the target compounds were determined by GC/MS in selective ion mode(SIM).The results showed a good linear relationship with correlation coefficients greater than 0.996 in range from 10 to 600μg/L.The detection limits of the compounds were from 0.10μg/kg to 0.31 μg/kg.And the recoveries of blank samples diatomite were between63.1%and86.7%,seven paralle samples were determined and the relative standard deviations were between 4.5% and 15.1%.The Three practical soil samples from yunnan were determined by using this method,PAHs and OCPs were detected,the PAHs residues ranged from 0.9×10^-3 mg/kg to 4.7×10^-3 mg/kg,the OCPs residues ranged from 0.8×10^-3 mg/kg to 6.6×10^-3 mg/kg.The method is suitable for the determination of PAHs and OCPs in soil.