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[目的]采用分散液相微萃取(DLLME)与气相色谱-火焰光度检测(GC-FPD)联用技术建立快速测定水体中毒死蜱和甲基对硫磷残留的新方法。[方法]分别考察萃取剂和分散剂种类与体积、萃取时间、离心时间和盐度等因素对萃取效果的影响,确立最佳萃取条件,采用外标法定量,在0.1~10mg/L范围内线性关系良好,相关系数为0.999。[结果]在最佳萃取条件下,毒死蜱和甲基对硫磷的平均添加回收率分别为104.10%、100.62%,平均富集系数分别为487.07、456.06,变异系数在2.23%~5.33%之间,仪器检出限在15~18 ng/g之间。[结论]该方法简便、快速、准确、重复性好,适用于水体中农药残留分析。
[Objective] The research aimed to establish a new method for rapid determination of chlorpyrifos and methyl parathion residue in water by using liquid chromatography coupled with liquid chromatography-flame photometry (DLL-FPME). [Method] The effects of the factors such as the type and volume of extractant and dispersant, extraction time, centrifugation time and salinity on the extraction were investigated. The optimal extraction conditions were established. The external standard method was used to determine the optimum extraction conditions. The optimum extraction conditions were 0.1-10mg / L The linearity is good with a correlation of 0.999. [Result] Under the optimal extraction conditions, the average recoveries of chlorpyrifos and methyl parathion were 104.10% and 100.62%, respectively. The average enrichment coefficients were 487.07 and 456.06, respectively, and the coefficients of variation were between 2.23% and 5.33% , The detection limit of the instrument is between 15 ~ 18 ng / g. [Conclusion] The method was simple, rapid, accurate and reproducible. It was suitable for the analysis of pesticide residues in water.