建立了一种测定甘蔗和土壤中敌草隆农药残留的超高效液相色谱(UPLC)方法。样品经水和甲醇提取,二氯甲烷液-液分配后,过中性氧化铝柱纯化,用石油醚:乙酸乙酯的混合液(体积比85:15)淋洗和洗脱,洗脱液经减压浓缩后用5mL乙腈定容。采用UPLC分离,紫外检测器检测,外标法定量。敌草隆在0.02~5.0mg/L范围线性关系良好,相关系数为0.9999;甘蔗、土壤和甘蔗叶中敌草隆的平均回收率分别为76.0%~98.4%、84.1%~98.0%和79.2%~90.0%;变异系数分别为0.69%~2.93%、5.11%~9.30%和2.45%~4.92%。检出限分别为5μg/kg、10μg/kg和10μg/kg。
A method based on ultra performance liquid chromatography(UPLC) has been developed for the determination of diuron residues in sugar cane and soil.The samples were extracted with water and methanol,distributed by dichloromethane liquid-liquid extraction,and then purified by alumina column.After washing and eluted with petroleum ether and ethyl acetate(85:15,V/V),the eluate was evaporated to dryness by rotary evaporation,and then dissolved in 5 mL acetonitrile.The residues were determined by ultra performance liquid chromatography and quantified by external standard method.The linear ranges were 0.02~5.0 mg/L for diuron.The detection limit were 5 μg/kg in sugar cane,10 μg/kg in soil and 10 μg/kg in sugar cane leaf.The average recoveries in spiked sample were 76.0%~98.4% for sugar cane,84.1%~98.0% for soil and 79.2%~90.0% for sugar cane leaf.