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[方法]样品用乙腈提取,弗罗里硅土固相萃取小柱净化,高效液相色谱仪分离,紫外234、281 nm分别检测虫酰肼和辛硫磷,外标法定量。[结果]对大白菜和土壤中的虫酰肼、辛硫磷进行不同水平的添加回收率试验,方法的平均回收率为77.18%~107.27%,相对标准偏差为1.50%~8.83%。虫酰肼在大白菜和土壤中的最低检测质量分数为0.01 mg/kg,辛硫磷在大白菜和土壤中的最低检测质量分数为0.02 mg/kg。[结论]该方法的灵敏度、准确度、精密度符合农药残留分析的要求,适合大批量样品的检测。
[Method] The samples were extracted with acetonitrile, purified with Florisil solid-phase extraction cartridges, and separated by high performance liquid chromatography. The contents of insects hydrazide and phoxim were detected by UV at 234 and 281 nm, respectively. [Result] The recoveries of different levels of tebufenozide and phoxim in Chinese cabbage and soil were tested. The average recoveries were 77.18% ~ 107.27% and the relative standard deviations were 1.50% ~ 8.83%. The minimum detectable mass fraction of tebufenozide in Chinese cabbage and soil was 0.01 mg / kg, while the minimum detectable mass fraction of phoxim in Chinese cabbage and soil was 0.02 mg / kg. [Conclusion] The sensitivity, accuracy and precision of the method met the requirements of pesticide residue analysis and was suitable for the detection of large quantities of samples.