微波萃取-固相萃取净化-气相色谱法测定土壤中有机氯农药  

Determination of Organochlorine Pesticides in Soil by Gas Chromatographic with Microwave Extraction and Solid Phase Extraction Purification

作　　者：李敬玖 谢洪勇[1] 王婕[1] 孙志国[1] 陈卫东 李强 

机构地区：[1]上海第二工业大学环境与材料工程学院,上海201209 [2]上海华测品标检测技术有限公司,上海201206

出　　处：《上海第二工业大学学报》2016年第1期32-36,共5页Journal of Shanghai Polytechnic University

基　　金：上海自然科学基金项目(No.15ZR1416900)资助

摘　　要：采用微波萃取-固相萃取(SPE)净化-气相色谱法测定土壤中21种痕量半挥发性有机氯农药(OCPs)。以丙酮-正己烷(体积比为1:1)作为萃取溶剂,所得萃取液浓缩至1 m L,通过CARB/NH2固相萃取柱进行纯化。用丙酮-正己烷(体积比为1:4)混合溶剂将有机氯农药从萃取柱中洗脱,洗脱液浓缩至1 m L后用气相色谱法测定。加入标样对OCPs进行回收,回收率在72%～109%之间,测定值的相对标准偏差(n=6)均小于5%。测得21种OCPs的检出限在0.05～0.5μg/kg之间。实际土壤样品的测定结果表明:α-六六六(含量为0.15～0.16μg/kg)、β-六六六(含量为0.32～1.07μg/kg)、β-硫丹(含量为0.20～0.23μg/kg)及异狄氏醛(含量为0.65μg/kg),均有少量检出。Twenty one organochlorine pesticides （OCPs） presented in soil as pollutants, were determined by gas chromatographic with microwave extraction and solid phase extraction （SPE）. Acetone and n-hexane （ratio in volume was 1 ： 1） was used as extraction solvent and the extract was concentrated to 1 mL, which was then purified on the solid phase extraction column and eluted from the column with mixed solvent of acetone and n-hexane （ratio in volume was 1 ： 4）. The eluate was concentrated to 1 mL and used for gas chromatography determination. Recovery was tested by addition of OCPs standards and the recovery rate ranged from 72% to 109%. Values of RSD＇s （n = 6） for all the 21 OCPs were less than 5%. Detection limits ranged from 0.05 to 0.5 μg/kg. The determination results of the soil samples showed that α-hexachlorocyclohexane,β-hexachlorocyclohexane,β-endosulfan and endrin were detected little with the content of 0.15～0.16 μg/kg, 0.32～1.07 μg/kg, 0.20～0.23 μg/kg and 0.65 μg/kg respectively.

关 键 词：有机氯农药 微波萃取 气相色谱 固相萃取 土壤 

分 类 号：X839.2[环境科学与工程—环境工程]