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建立了一种快速、灵敏、可靠的用于分析稻田环境中氯氟氰虫酰胺残留的方法,同时研究了氯氟氰虫酰胺在稻田环境中的消解特性。田间样品经液-液分配及优化的Qu ECh ERS方法提取及净化,采用超高效液相色谱-串联质谱法(UPLC-MS/MS)进行定性、定量分析。结果表明:添加水平分别在0.002~0.5 mg/kg下,氯氟氰虫酰胺在稻田水、土壤以及水稻植株空白样品中的平均添加回收率为70%~101%,相对标准偏差(RSD,n=5)为0.7%~9.1%,其在田水、土壤和水稻植株中的最低检测浓度分别为0.002、0.005和0.01 mg/kg。该方法可满足水稻及其环境中氯氟氰虫酰胺残留量的检测要求。消解动态试验结果表明,氯氟氰虫酰胺在稻田水、土壤及水稻植株中的消解过程符合一级动力学方程,消解半衰期分别为4.8~7.7 d、5.2~8.3 d和1.5~15.4 d,属于易消解农药。
A fast, sensitive and reliable method for the analysis of flumethoxam residues in paddy field was established. Meanwhile, the digestion characteristics of flumethrin in rice field were also studied. Field samples were extracted and purified by liquid-liquid partitioning and optimized Qu ECh ERS method, and were characterized by UPLC-MS / MS. The results showed that the average recoveries of flumethoxamid from paddy soil, paddy soil and rice blank plants ranged from 70% to 101% with the addition levels of 0.002-0.5 mg / kg respectively. The relative standard deviations (RSD, n = 5) ranged from 0.7% to 9.1%. The lowest concentrations tested in field, soil and rice plants were 0.002, 0.005 and 0.01 mg / kg, respectively. The method can meet the detection requirements of amoxicclamide residue in rice and its environment. The dynamic test results of digestion showed that the degradation of flumethoxam in paddy field water, soil and rice plants was in accordance with the first-order kinetic equation with the half-lives of 4.8-7.7 days, 5.2-8.3 days and 1.5-15.4 days, respectively, belonging to Easy to digest pesticides.