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基于超声提取、磁性固相萃取技术,建立了土壤中四种苯脲类除草剂的前处理方法,并采用超高效液相色谱质谱法进行定性定量分析。优化了萃取溶剂、超声频率、萃取时间、初始超声萃取温度、稀释水样体积、磁性纳米材料的种类和用量对土壤中待测物质回收率的影响。在最佳优化条件下,待测物质的回收率为72.7%~94.4%,相对标准偏差(RSD)为3.4%~12%,线性范围为5~200μg/kg,检出限0.24~0.33μg/kg,该方法具有检出限低,灵敏度高等特点,适用于土壤中痕量苯脲类物质的测定。
Based on ultrasonic extraction and magnetic solid-phase extraction, four pre-treatment methods for the determination of four kinds of phenylurea herbicides in soil were established and characterized by ultra performance liquid chromatography-mass spectrometry. The effects of extraction solvent, ultrasonic frequency, extraction time, initial ultrasonic extraction temperature, dilution water sample volume, the type and amount of magnetic nanomaterials on the recovery of analytes in soil were optimized. Under the optimum conditions, the recoveries of the tested substances ranged from 72.7% to 94.4% with relative standard deviations (RSDs) of 3.4% ~ 12%. The linear range was 5 ~ 200μg / kg with the detection limit of 0.24 ~ 0.33μg / kg. The method has the advantages of low detection limit, high sensitivity and is suitable for the determination of traces of phenylureas in soil.