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固相萃取-气相色谱法测定土壤中多种持久性有机污染物
Solid-phase Extraction and Gas Chromatography Determination of Persistent Organic Pollutants in soil
【Author】 LI Dong-mei~(1,2),LI Jian-ke~(1*),SHI Zhi-cheng~3,LI jun-jian~2 (1 College of Food Science,Shaanxi Normal University,Xi’an 710069,China; 2 Xi’an Agriculture Science Research Institute,Xi’an 710061,China; 3 College of Life Science,Northwest University,Xi’an 710069,China)
【机构】 陕西师范大学食品工程与营养科学学院; 西安市农业科学研究所; 西北大学生命科学学院;
【摘要】 目的建立土壤中的持久性有机污染物(POPs)残留测定方法。方法以正己烷和丙酮为溶剂、超声波提取、弗罗里硅土固相萃取小柱净化、大口径石英玻璃毛细管柱分离和微池电子捕获检测器气相色谱法检测。结果 14种POPs在22分钟之内很好分离,方法检出限为0.0048~0.0378 ng/g,空白加标回收率为73.1%~11 1.9%,样品加标回收率为67.9%~124.6%,相对标准偏差为2.02%~6.26%。对菜地和茶园两种不同利用方式的土壤进行测定,14种POPs在两种土壤中均有检出,主要残留物都是DDTs、异狄氏剂及七氯。菜地土壤DDTs残留显著高于茶园,其它残留值相似,值都较低。结论该方法可满足痕量POPs的测定要求,为环境样品的检测提供科学的方法和依据。
【Abstract】 Aim To setup an efficient method for determination organophosphate pesticides of POPs in soils.Methods The POPs were extracted and associated with ultrasonic treatment from soil samples with n-hexane and acetone and cleaned up by Florisil solid-phase extraction column.Then,the extract was separated by big caliber capillary column and detected by GC withμECD detector.Results Fourteen POPs were separated in 22 minutes.The MDLs are 0.0048~0.0378 ng/g,the average recoveries for spiked standards in samples are 67.9%~124.6%,the relative standard deviations are 2.02%~6.26%.Residual levels of Fourteen POPs in defferent soils were also analyzed.The result shows that fourteen POPs were 100%detected in six samples.DDTs,Endrin and Heptachlor are the main residues.The average levels of DDTs in vegetable base were prominently higher than in tea plantation.Conclusion The method can meet the needs of determination of trace amount POPs soil. POPs are still potentially pollutants for agricultural environment.
【Key words】 Solid-phase Extraction; Gas Chromatography; soil; Persistent Organic Pollutants(POPs);
- 【会议录名称】 2008陕西省环境与健康论坛论文集
- 【会议名称】2008陕西省环境与健康论坛
- 【会议时间】2008-08-01
- 【会议地点】中国陕西西安
- 【分类号】X833
- 【主办单位】陕西省环境保护局、陕西省卫生厅、陕西省毒理学会、西北大学生命科学学院、中国毒理学会毒理学史专业委员会