土壤中6种氯代多环芳烃测定方法的建立及应用

原文婷<sup>1</sup>; 高占啟<sup>2</sup>; 孙成<sup>1*</sup>

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 Cheng^1,2

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 PAH^s） 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 MP^a 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 PAH^s， 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 PAH^s in the soil of a chemical park.

Key words: Accelerated solvent extraction Gel permeation chromatography Cl-PAH^s Soil