QuEChERS-高效液相色谱法测定土壤中嘧霉胺和吡唑醚菌酯残留

Simultaneous Determination of Pyrimethanil and Pyraclostrobin Residues in Soil by QuEChERS Pretreatment Combined with High Performance Liquid Chromatography

[目的]建立一种QuEChERS样品前处理联合高效液相色谱-二极管阵列(HPLC-PDA)同时测定土壤中嘧霉胺和吡唑醚菌酯残留量的分析方法。[方法]采用QuEChERS方法对土壤样品进行前处理,以乙腈作为提取剂,PSA+C18+无水Mg SO4净化,HPLC-PDA检测,外标法定量。[结果]嘧霉胺和吡唑醚菌酯的最低检出限分别为6.2、12.8μg/L,定量限分别为19.6、37.7μg/L,在3个农药添加水平下(100、400、800μg/kg)嘧霉胺及吡唑醚菌酯的回收率范围为86.3%~99.2%,相对标准偏差为2.0%~5.4%。[结论]该方法准确、快速、方便,适用于土壤中嘧霉胺、吡唑醚菌酯这2种杀菌剂农药的残留检测。

[Aims] An analytical method for the simultaneous determination of pyrimethanil and pyraclostrobin residues in soil by QuEChERS pretreatment combined with high performance liquid chromatography-diode array detector（HPLC-PDA） was developed. [Methods] The soil samples were pretreated by QuEChERS method, extracted with acetonitrile, and then the extractant was purified with the mixture of PSA, C18 and anhydrous Mg SO4. The target compounds were analyzed by high performance liquid chromatography equipped with diode array detector and quantified by external standard method. [Results] The limits of detection for pyrimethanil and pyraclostrobin were 6.2and 12.8 μg/L, and the limits of quantitation were 19.6 and 37.7 μg/L, respectively. When the stiked levels were 100,400 and 800 μg/kg, the recoveries ranged from 86.3 to 99.2% with the relative standard deviations of 2.0-5.4%.[Conclusions] The method is accurate, rapid and convenient, which is suitable for the detection of pyrimethanil and pyraclostrobin in soil.