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建立了同时检测对土壤中磺胺脒、磺胺嘧啶、磺胺甲恶唑、烯啶虫胺、吡虫啉、噻虫啉、多菌灵7种农药残留的在线净化-双检测器-高效液相色谱新方法。实验对提取净化和分析条件进行了优化,得出最佳实验条件:土壤样品经提取液(甲醇:乙腈:二氯甲烷=5:4:1,V/V/V)提取,氮吹浓缩后直接进样,经在线固相萃取(SPE)柱在线净化,梯度洗脱经反相C18色谱柱分离,二极管阵列(DAD)检测器串联荧光(FLD)检测器检测,外标法定量,12 min内即可完成7种农兽药的检测。7种农药检出限为1.1~3.0×10~(-3)mg/kg(S/N=3),线性范围内线性相关系数均在0.9999以上。空白土壤样品在0.05,0.10,0.32 mg/kg添加水平的平均加标回收率为71.92%~103.88%,相对标准偏差为0.07%~4.1%。
A new method for on-line decontamination of seven kinds of pesticide residues in soil, such as sulfadiazine, sulfadiazine, sulfamethoxazole, nitenpyram, imidacloprid, thiacloprid and carbendazim, was established . In the experiment, the conditions of extraction and purification and analysis were optimized, and the optimum experimental conditions were obtained. The soil samples were extracted with the extract (methanol: acetonitrile: dichloromethane = 5: 4: 1, V / V / V) The sample was directly injected into the column and purified by on-line solid-phase extraction (SPE) column. The column was eluted with reversed-phase C18 column. The detector was detected by diode array (DAD) Within seven kinds of pesticides to complete the test. The detection limits of seven pesticides ranged from 1.1 to 3.0 × 10 -3 mg / kg (S / N = 3), and the linear correlation coefficients were above 0.9999 in the linear range. The average spike recoveries of blank soil samples at the addition levels of 0.05, 0.10 and 0.32 mg / kg ranged from 71.92% to 103.88% with relative standard deviations of 0.07% -4.1%.