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

作　　者：张卢军[1] 潘灿平[1] 郝向红[1] 赵玉珍[1] 马婧玮[1] 宗伏霖[2] 

机构地区：[1]中国农业大学理学院,北京100094 [2]农业部农药检定所,北京100026

出　　处：《农药学学报》2007年第1期100-102,共3页Chinese Journal of Pesticide Science

基　　金：全球环境保护基金项目--GEF项目(GF/CPR/04/002)

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。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 （ R^2 = 0. 999 5 ）. The limit of detection （LOD） of this method is 0.3 txg/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.

关 键 词：六氯苯 气质联机 逆固相基质分散净化 土壤 

分 类 号：S481.8[农业科学—农药学] O657.71[农业科学—植物保护]