高效液相色谱-三重串联质谱法同时检测稻田中阿维菌素与茚虫威的残留量  

Simultaneous Determination of Abamectin and Indoxacard Residues in Paddy Fields by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：侯志广[1] 方永睿 嘧东林 张浩[1] 赵晓峰[1] 王鑫宏[1] 逮忠斌[1] 

机构地区：[1]吉林农业大学资源与环境学院,长春130118 [2]济南市历城区环境保护局,济南250100

出　　处：《农药》2015年第10期744-747,共4页Agrochemicals

基　　金：农业部农药残留项目(2012P179);吉林省科技厅青年基金资助(2010-0142)

摘　　要：[目的]明确阿维菌素、茚虫威及二者的复配制剂在稻田施用后,其有效成分阿维菌素B1a、阿维菌素B1b和茚虫威在稻田植株上的消解趋势、糙米中的残留水平。[方法]建立了高效液相色谱-三重串联质谱法HPLC-MS/MS(ESI+)同时检测稻田植株、稻田土壤、稻田水、稻壳以及糙米5种基质中阿维菌素与茚虫威残留量的分析方法。[结果]阿维菌素B1a和茚虫威均在0.002~1 mg/L范围内线性关系良好。二者在5种基质中0.01、0.02、0.2 mg/L添加水平的回收率分别为71.2%~102.0%、72.6%~106.3%,变异系数分别为1.4%~13.2%、2.6%~19.1%(n=5)。阿维菌素B1b在0.001~0.05 mg/L范围内线性关系良好,在0.000 4、0.004、0.04 mg/L三个添加水平的平均回收率为78.0%~101.7%,变异系数为2.6%~20.8%(n=5)。阿维菌素B1a、阿维菌素B1b和茚虫威的检出限分别为0.2、0.004、0.2μg/kg,定量限分别为0.01、0.000 4、0.01 mg/kg。方法的准确度、精密度满足农残检测的要求。采用该方法对施药后的水稻取样检测,144份糙米中阿维菌素与茚虫威的残留量均低于检出限。[结论]该方法简便、灵敏、节约成本,可用于水稻中农药多残留的快速检测。[Aims] The dissipation dynamics of avermectin BI~, avermectin Bib and indoxacard in paddy plant and the final residues in brown rice were studied after avermectin, indoxacard and avermectin .indoxacard 7.6% ME were applied. [Methods] A novel method for simultaneous determination ofavermeetin and indoxacard residues in paddy plant, paddy soil, paddy water, rice hull and brown rice by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was studied. [Results] The results showed that the linear relation were good when the concentrations of avermectin Bla and indoxacard were in the range of 0.002-1 mg/L. When the addition levels were 0.01, 0.02, 0.2 mg/kg, the recoveries of avermectin B~, and indoxacard were 71.2-102.0% and 72.6-106.3%, the range of relative standard deviation （RSD） were 1.4-13.2% and 2.6-19.1%, respectively. There was a good linear relation when the concentrations of avermectin Bib was in the range of 0.001-0.05 mg/kg. When the addition levels were 0.000 4, 0.004 and 0.04 mg/kg, the average recoveries of avermectin Bib in five matrix were ranged from 78.0-101.7% and the RSD were between 2.6 and 20.8%. The limits of detection （LOD） of avermectin B~, avermectin Bt~ and indoxacard were 0.2, 0.004 and 0.2 p^g/kg while limits of quantification （LOQ） were 0.01, 0.000 4 and 0.01 mg/kg, respectively. In addition, this method was successfully used for the study on 144 brown rice samples which were sprayed with abamectin and indoxacard in rice growth period. The results showed that the final residues of them were no detected. [Conclusions] The method was simple, sensitive and economical, which can meet the requirements for simultaneous determination of many pesticides in rice.

关 键 词：阿维菌素 茚虫威 高效液相色谱-三重串联质谱 残留 稻田 

分 类 号：S481.8[农业科学—农药学] O657.63[农业科学—植物保护]