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当前位置: 首页 > 文章 > 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 农药学学报 2007,9 (1) 100-102
Position: Home > Articles > Determination of Hexachlorobenzene in Soils by Dispersive Solid-phase Extraction and Gas Chromatography-mass Spectrometry 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

作  者：
张卢军;潘灿平;郝向红;赵玉珍;马婧玮;宗伏霖
单  位：
农业部农药检定所;中国农业大学理学院
关键词：
六氯苯;气质联机;逆固相基质分散净化;土壤
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0.05～5mg/L浓度范围内呈现出较好的线性关系,相关系数R2=0.9995;方法检测限为0.3μg/kg,定量限为0.9μg/kg,在0.89、1.78、8.90mg/kg3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1～10m深的土壤样本,发现六氯苯的残留量在2.3～25912mg/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。
译  名：
Determination of Hexachlorobenzene in Soils by Dispersive Solid-phase Extraction and Gas Chromatography-mass Spectrometry
作  者：
ZHANG Lu-jun1, PAN Can-ping1, HAO Xiang-hong1, ZHAO Yu-zhen1,MA Jing-wei1, ZONG Fu-lin2(1.College of Sciences,China Agricultural University,Beijing 100094,China;2.Institute of the Control of Agrochemicals,Ministry of Agriculture,Beijing 100026,China)
关键词：
hexachlorobenzene;gas chromatography-mass spectrometry;PSA; soil
摘  要：
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 soilsurface 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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