土壤中拟除虫菊酯类残留农药的气相色谱测定方法研究  

DETERMINATION OF RESIDUES OF PYRETHROID INSECTICIDES IN SOIL BY CAPILLARY GAS CHROMATOGRAPHY

作　　者：陈莉[1] 章钢娅[2] 靳伟[2] 胡锋[1] 

机构地区：[1]南京农业大学资源与环境科学学院,南京210095 [2]中国科学院南京土壤研究所,南京210008

出　　处：《土壤学报》2006年第5期764-771,共8页Acta Pedologica Sinica

基　　金：国家重点基础研究发展规划(973)项目(2002CB410805)资助

摘　　要：建立了土壤中氯氰菊酯、氰戊菊酯和溴氰菊酯的提取、净化以及毛细管气相色谱的测定方法。运用石油醚-丙酮（P／P，2：1）混合溶剂提取，用氟罗里硅土进行层析净化，60ml石油醚／乙酸乙酯（V／V，9：1）进行洗脱，电子捕获-气相色谱测定，单点外标法定量。实验表明：土样中添加0．08mgkg^-1的氯氰菊酯、氰戊菊酯和溴氰菊酯3种农药混标时，方法回收率为89．67％～90．62％，添加0．40mgkg^-1时．方法回收率为91、07％～93．02％；操作中相对标准偏差（RSD）为2．02％～3．70％，最小检出量可达1．00pg。在检测色谱精密度实验中，5次测定3种农药混标，相对标准偏差（RSD）为1．37％～2．88％。实验表明，该法具有灵敏度高、操作简便、净化效果好、重现性好等特点。A method for extracting, clearing off and determining residues of cypermethrin, fenvalerate and deltamethrin in soil has been developed. The method uses pertole mether-acecton （ V/ V, 2 ： 1 ） mixture to extract residues of the pesticides in soil samples, a column （20 cm × 1.5 cm） packed with 3 g Florisil to clear the mixture of the residues, and pertolem ether-ethyl acetate （ V/V, 9：1 ） to elute the residues from the column. Then the eluent is determined by gas chromatography （ECD-GC） with a HP-5 （30 m × 0.32 mm × 0.25 μm） capillary column and quantified by the single pointexternal standard method. In an experiment of using this method, the recovery rates of cypermethrin, fenvalerate and dehamethrin were found to be 90.10% 93.02%, 90.62%- 91.07% and 89.67%- 91.53% respectively with RSD being2.02%- 2.49%, 2.51%- 3.70% and 3.08% - 3.42%, respectively in the operation. And the minimum detectable quantity was 1.00 pg. The relative standard deviations （ n = 5） of the equipment ranges from 1.37% to 2.88%. This method is proved to be easy in operation, and high in sensitivity, reproductivity and selectivity.

关 键 词：土壤 拟除虫菊酯 残留量 气相色谱法 

分 类 号：X131.3[环境科学与工程—环境科学]