张卢军, 潘灿平, 郝向红, 赵玉珍, 马婧玮, 宗伏霖. 逆固相基质分散净化和气质联机检测土壤中的六氯苯残留[J]. 农药学学报, 2007, 9(1): 100-102.
    引用本文: 张卢军, 潘灿平, 郝向红, 赵玉珍, 马婧玮, 宗伏霖. 逆固相基质分散净化和气质联机检测土壤中的六氯苯残留[J]. 农药学学报, 2007, 9(1): 100-102.
    ZHANG Lu-jun, PAN Can-ping, HAO Xiang-hong, ZHAO Yu-zhen, MA Jing-wei, ZONG Fu-lin. Determination of Hexachlorobenzene in Soils by Dispersive Solid-phase Extraction and Gas Chromatography-mass Spectrometry[J]. Chinese Journal of Pesticide Science, 2007, 9(1): 100-102.
    Citation: ZHANG Lu-jun, PAN Can-ping, HAO Xiang-hong, ZHAO Yu-zhen, MA Jing-wei, ZONG Fu-lin. Determination of Hexachlorobenzene in Soils by Dispersive Solid-phase Extraction and Gas Chromatography-mass Spectrometry[J]. Chinese Journal of Pesticide Science, 2007, 9(1): 100-102.

    逆固相基质分散净化和气质联机检测土壤中的六氯苯残留

    Determination of Hexachlorobenzene in Soils by Dispersive Solid-phase Extraction and Gas Chromatography-mass Spectrometry

    • 摘要: 建立了逆固相基质分散净化和气质联机法(GC-MS)快速、简便测定土壤中六氯苯(HCB)残留量的方法。以丙酮-正己烷(1∶ 1,体积比)为提取剂,采用超声波萃取,经固相基质PSA(primary secondary amine)吸附净化后采用GC-MS选择离子模式检测。结果表明,六氯苯在0.05~5 mg/L浓度范围内呈现出较好的线性关系,相关系数R2=0.999 5; 方法检测限为0.3 μg/kg,定量限为0.9 μg/kg,在0.89、1.78、8.90 mg/kg 3个添加水平上的平均回收率分别为106.6%、108.2%和108.1%。用该方法测定了天津某生产厂厂区地下1~10 m深的土壤样本,发现六氯苯的残留量在2.3~25 912 mg/kg 之间,表现出显著的空间变异趋势。该方法快速、简便、经济、高效、实用并且安全,适合大批量样本中六氯苯的快速检测。

       

      Abstract: A quick,easy,cheap,effective,rugged and safe method was improved to analyze hexachlorobenzene (HCB) residues in soils by dispersive solid-phase extraction and gas chromatography-mass spectrometry (GC-MS).HCB residues in soils was extracted with acetone/hexane (1∶ 1,v/v) under ultrasonic extraction,and cleaned up on primary secondary amine (PSA) by removing the polar matrix components or interferences.GC-MS was then used for quantitative and confirmatory analysis of HCB.Linear calibration curves were obtained for HCB with a concentration range of 0.05~5 mg/L (R2=0.999 5).The limit of detection (LOD) of this method is 0.3 μg/kg,LOQ is 0.9 μg/kg.Recoveries of 106.6%,108.2%和108.1% have been achieved at three concentrations of 0.89,1.78 and 8.90 mg/kg,respectively.Using this method we got the information of HCB residue in the soils from HCB manufacturing factories.The sample sites were below the soil surface from depth of 1 m to 10 m.The results showed the concentration of HCB in the soils at the residue levels from 2.3 mg/kg to 25 912 mg/kg.Most concentrations of these HCB samples exceeded the MRLs of HCB for agricultural soils.

       

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