超高效液相色谱-串联质谱法(UPLC-MS/MS)快速检测小麦和土壤中氟环唑的残留及消解

Determination of Epoxiconazole in Wheat and Soil Using Ultra-Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry(UPLC-MS/MS)

为了解氟环唑在小麦和土壤中的消解动态,建立了超高效液相色谱-串联四级杆质谱(UPLC-MS/MS)快速检测小麦及土壤中氟环唑残留的分析方法,并在山东、河南和北京开展了为期两年的小麦田间试验研究。不同浓度氟环唑(0.05、0.5、1.0mg·kg-1)的添加回收率试验结果表明:在土壤中平均回收率为98.8%～108.1%,变异系数为2.6%～6.7%;在小麦植株中的平均回收率为73.2%～84.4%,变异系数为0.9%～4.6%;在小麦粒中的平均回收率为80.7%～82.4%,变异系数为2.0%～7.8%。氟环唑在山东、河南和北京三地的小麦和土壤中的消解动态研究结果表明,氟环唑在土壤中的消解半衰期分别为16.9、21.3、19.7d,在小麦植株上的半衰期分别为12.6、9.2、8.1d,属于易降解农药。

In order to know the degradation of epoxiconazole in wheat and soil clearly,a sensitive and effective method for the determination of epoxiconazole in wheat and soil using ultra-high performace liquid chromatograph（UPLC-MS/MS） was established.Moreover,the degradation of epoxiconazole in wheat and soil in Shandong,Henan and Beijing Provinces was also investigated.The epoxiconazole residues were analyzed by UPLC-MS/MS under multiple reaction monitoring mode.The average recoveries using this method at three spiking levels（0.05 mg·kg-1,0.5 mg·kg-1,1.0 mg·kg-1） were also evaluated.The results indicated that recoveries ranged from 98.8% to 108.1% with variation coefficient（CV） in the range of 2.6%～6.7%（n=5） in soil,from 73.2%～84.4% with CV of 0.9%～4.6% in wheat plant and from 80.7%～82.4% with CV of 2.0%～7.8% in wheat,respectively.Meanwhile,a field experiment was also conducted to reveal the dynamics of epoxiconazole residues in wheat and soil in the three provinces.The results showed that the half life of epoxiconazole was 16.9 days,21.3 days,19.7 days in soil and 12.6 days,9.2 days,8.1 days in wheat plant in Shandong,Henan and Beijing respectively which showed that epoxiconazole belonged to non-persistent and easily degradable pesticide.