高效液相色谱法测定土壤中辛硫磷

Detection of Phoxim in Soil by High Performance Liquid Chromatography

[目的]建立振荡溶剂萃取-高效液相色谱法测定土壤中辛硫磷农药残留量方法。[方法]在振荡萃取试验条件优化的基础上,确定最佳试验条件。[结果]最佳试验条件为:以二氯甲烷∶丙酮(7∶3)为萃取溶剂,振荡30 min,循环2次。萃取液经弗罗里硅土小柱净化后,氮吹到1 ml,于高效液相色谱测定。辛硫磷的线性范围在0.15～10.0μg/ml,相关系数为0.999 4,最低检测限为15.8μg/kg,精密度(n=6)为0.39%。实际样品3个添加水平(100、200、500μg/kg)下得到回收率为82.8%～90.6%。[结论]该方法具有较好的灵敏度和准确性。

[Objective] A method was described for the determination of phoxim in soil by high performance liquid chromatography with oscillation solvent extraction.[Method]The experimental conditions were investigated on the basis of the optimization of condition.[Result] The optimal conditions were obtained as follows： extraction solvent dichloromethane∶ acetone=7∶3,extraction time 30 min,cycling twice.The extract was cleaned up by florisil.The lute was evaporated to dryness under nitrogen to 1.0 ml and the quantitative analysis of phoxim was performed by HPLC.The linear range was 0.15-10.0 μg/ ml,the detection limits was 15.8 μg/kg,the relative standard deviations was 0.39%（n=6）.The average recoveries spiked at the levels of 100,200,500 μg/kg ranged from 82.8% to 90.6% of soil samples.[Conclusion] The method has good sensitivity and accuracy.