引用本文:原文婷,高占啟,孙成.土壤中6种氯代多环芳烃测定方法的建立及应用[J].环境监控与预警,2015,7(6):14-20
YUAN Wen ting, GAO Zhan qi, SUN Cheng.Method Development and Application for the Determination of Chlorinated Polycyclic Aromatic Hydrocarbons in Soil[J].Environmental Monitoring and Forewarning,2015,7(6):14-20
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土壤中6种氯代多环芳烃测定方法的建立及应用
原文婷,高占啟,孙成1,2
1.污染控制与资源化研究国家重点实验室,南京大学环境学院,江苏 南京 210023;2.国家环境保护地表水环境有机污染物检测分析重点实验室,江苏省环境监测中心,江苏 南京 210036
摘要:
建立了加速溶剂萃取、凝胶渗透色谱(GPC)与气相色谱-质谱联用测定土壤中6种氯代多环芳烃的分析方法。研究证实该法的最佳萃取条件为:10.34 MPa压力,100 ℃萃取温度下,以1∶1(V/V)的正己烷/二氯甲烷为萃取溶剂,静态萃取10 min,循环4次。GPC净化过程用乙酸乙酯和环己烷的混合液1∶1(V/V)做洗脱液,目标物的收集时间为25~35min。方法对Cl-PAHs在1~500 μg/L范围内线性良好,相关系数R2为0.998 4~0.999 7;LOD和LOQ分别为2.6~25.1 pg/g和8.7~83.6 pg/g;各目标物的低浓度回收率为64.1%~117.6%,RSD<12.05%;高浓度回收率为59.1%~105.3%,RSD<9.81%。研究证实该法满足定量分析的要求,并应用该法对某化工园进行了氯代多环芳烃的检测。
关键词:  加速溶剂萃取  凝胶渗透色谱  氯代多环芳烃  土壤
DOI:
分类号:X833
基金项目:江苏省环境监测科研基金资助项目(1208)
Method Development and Application for the Determination of Chlorinated Polycyclic Aromatic Hydrocarbons in Soil
YUAN Wen ting, GAO Zhan qi, SUN Cheng1,2
1.State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing, Jiangsu 210023, China;2. State Environmental Protection Key Laboratory of Monitoring and Analysis for Organic Pollutants in Surface Water, Environment Monitoring Center of Jiangsu Province, Nanjing, Jiangsu 210036, China
Abstract:
A method was developed for the determination of 6 chlorinated polycyclic aromatic hydrocarbons (Cl PAHs) in soil by accelerated solvent extraction (ASE), gel permeation chromatography (GPC) coupled with GC MS. The optimal ASE efficiency was obtained when using 1:1(V:V) dichloromethane/n hexane as the extraction solvent, and performing the static extraction under 10.34 MPa pressure for 10 min at 100 ℃ for four times repeatedly. The obtained extract was passed through GPC to clean up and eluted with 1∶1 (V: V) cyclohexane/ethyl acetate. The fraction was collected between 25 and 35 min. Good linearity was observed in the range of 1 to 500 μg/L of Cl PAHs, with correlation coefficients varying from 0.9984 to 0.9997. The limits of detection and limits of quantification were 2.6~25 pg/g and 8.7~83.6 pg/g, respectively. The recoveries for the studied Cl PAHs ranged from 64.1% to 117.6% with the relative standard deviations less than 12.05% when the spiked concentration was low. When the spiked concentration was high, the recoveries ranged from 59.1% to 105.3% with the relative standard deviations less than 9.81%. This method was shown to meet the requirement for quantification analysis. It was applied in the determination of Cl PAHs in the soil of a chemical park.
Key words:  Accelerated solvent extraction  Gel permeation chromatography  Cl-PAHs  Soil