作　　者： (陈莉）; (刘冰洁）; (贾春虹）; (余苹中）; (贺敏）; (赵尔成）; (靖俊杰）;

机构地区： 北京市农林科学院植物保护环境保护研究所,北京100097

出　　处： 《农药》 2017年第8期593-595,602,共4页

摘　　要： [目的]建立测定姜和土壤中乙氧氟草醚残留的QuEChERS-超高效液相色谱串联质谱(UPLC/MS/MS)方法,通过田间试验研究了乙氧氟草醚在姜田中的残留及消解动态。[方法]样品经乙腈涡旋提取5 min,上清液加入含PSA+C18填料的小离心管中,涡旋、离心净化后,采用UPLC/MS/MS测定。[结果]在0.001~0.5 mg/L范围内,乙氧氟草醚的进样质量浓度与其对应的峰面积间呈良好的线性关系,相关系数r=0.9999,该方法检出限(LOD)为0.001 mg/kg,最低检出质量分数(LOQ)为0.01 mg/kg。在0.01、0.05、0.1 mg/kg的添加水平下,乙氧氟草醚在姜中的平均回收率为82.0%~99.0%,相对标准偏差为5.04%~15.70%;在0.02、0.05、0.2 mg/kg的添加水平下,乙氧氟草醚在土壤中的平均回收率为90.1%~97.1%;相对标准偏差为1.95%~6.20%。[结论]乙氧氟草醚在土壤中的半衰期20.4~25.7 d;24%乙氧氟草醚乳油分别按照有效成分180、270 g a.i./hm2剂量于姜播后苗前开始施药,施药1次,姜收获时采样测定,乙氧氟草醚在姜中的残留量<0.01~0.0124 mg/kg,均小于欧盟规定的最大残留限量(MRL)0.05 mg/kg,因此,在姜田中使用乙氧氟草醚,有效剂量为180 g a.i./hm2,施药1次时,不会造成其在姜中残留超标的风险。 [Aims] An analysis method using QuEChERS-ultra performance liquid chromatography tandem mass spectrometry was developed for the determination of oxyfluorfen residues in ginger and soil. The residues and decline dynamics of oxyfluorfen in ginger field were conducted by field experiments. [Methods] The ginger and soil samples were extracted by QuEChERS with acetonitrile, cleaned up with PSA＋C18and detected by UPLC/MS/MS. [Results]When the concentration was in the range of 0.001 to 0.5 mg/L, the linear relationship between the mass concentration of oxyfluorfen and corresponding peak area was good, the linear correlation coefficient was 0.9999, the limit of detection（LOD） was 0.001 mg/kg, the limits of quantitation（LOQ） in those samples were 0.01 mg/kg. The average recoveries of oxyfluorfen in ginger samples at three spiked levels of 0.01, 0.05 and 0.1 mg/kg all ranged from 82.0 to 99.0% with the relative standard deviation（RSD） of 5.04-15.70%. The average recoveries of oxyfluorfen in soil samples at three spiked levels of 0.02, 0.05 and 0.2 mg/kg all ranged from 90.1 to 97.1% with the relative standard deviation（RSD） of 1.95 to 6.20%. [Conclusions] The half-lives of oxyfluorfen in soil were 20.4 to 25.7 d. The oxyfluorfen 24% EC was sprayed on soil at the dosage of 180 and 270 g a.i./ha for 1 time before the ginger emergence. The samples were collected at harvest, the residues of oxyfluorfen in ginger were 0.01-0.0124 mg/kg, which was less than the maximum residue limit（MRL） of 0.05 mg/kg stipulated by EU. Therefore, when oxyfluorfen was used in the ginger field at the dose of 180 g a.i./ha for 1 time, it will not cause the risk of excessive residue in ginger.

关 键 词： 乙氧氟草醚 姜 超高效液相色谱串联质谱 残留动态 土壤