环境化学

  • 许桂苹,欧小辉,梁柳玲,秦旭芝.加速溶剂萃取-固相萃取及铜粉净化技术在土壤有机氯农药分析中的应用[J].环境科学学报,2010,30(11):2250-2255

  • 加速溶剂萃取-固相萃取及铜粉净化技术在土壤有机氯农药分析中的应用
  • Application of accelerated solvent extraction, purification by solid phase extraction and copper powder desulfurization in the analysis of organochlorine pesticides in soil
  • 基金项目:广西科学研究与技术开发计划项目(桂科攻-0779011)
  • 作者
  • 单位
  • 许桂苹
  • 广西壮族自治区环境监测中心站, 南宁 530022
  • 欧小辉
  • 广西壮族自治区环境监测中心站, 南宁 530022
  • 梁柳玲
  • 广西壮族自治区环境监测中心站, 南宁 530022
  • 秦旭芝
  • 广西壮族自治区环境监测中心站, 南宁 530022
  • 摘要:对比了索氏提取、超声提取和加速溶剂萃取样品前处理方法在土壤中有机氯农药的萃取效果,首次采用两级温度相结合的加速溶剂萃取方式,兼顾不同挥发性萃取物的萃取效果,建立了土壤中有机氯农药的加速溶剂萃取样品前处理方法.萃取液经无水硫酸钠脱水、Florisil柱脱色和铜粉除硫后,进色谱分析,目标组分能有效避免杂质干扰,实现基线分离.实验结果表明,在优化条件下,8种有机氯农药检出限在0.05~0.20μg·kg-1之间,空白加标回收率为74.9%~124.8%,RSD为3.1%~8.8%;标准样品实验中,α-HCH及DDTs均在标准值范围内,加标回收率在78.5%~117.9%之间.
  • Abstract:Amethod for sample pretreatment of organochlorine pesticides in soil by accelerated solvent extraction (ASE),with two-stage extraction temperature,prior to gas chromatography was developed.The samples were extracted with a mixture of n-hexane and acetone (1:1,V:V) and the extracts were cleaned up on a Florisil solid phase extraction (SPE) cartridge and desulfurized with copper powder.The analyses were separated on a HP-5MS capillary column and detected with an electron capture detector.Validation of the technique was performed using standard reference materials.Recoveries for these matrices were good (78.5%~117.9%) with all RSDless than 10.7%.The method also was applied to real samples,and good linearity was obtained for 8 compounds with detection limits ranging from 0.05 μg·kg-1 to 0.20 μg·kg-1.Recoveries in spiked soil samples were 74.9%~124.8% with RSDof 3.1%~8.8%.

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