溴氰虫酰胺及其代谢物在辣椒和土壤中的残留降解研究  

Residue and Degradation of Cyantraniliprole and Its Main Metabolite in Pepper and Soil

作　　者：何红梅[1] 张春荣[1] 朱亚红[1] 张昌朋[1] 平立凤[1] 赵华[1] 吴珉[1] 汤涛[1] 蔡晓明[1] 李振[1] 

机构地区：[1]省部共建国家重点实验室培育基地“浙江省植物有害生物防控重点实验室”,农业部农药残留检测重点实验室,浙江省农业科学院农产品质量标准研究所,杭州310021

出　　处：《分析化学》2014年第8期1177-1182,共6页Chinese Journal of Analytical Chemistry

基　　金：分析测试科技计划项目(No.2013C37085);浙江省公益技术研究农业项目(No.2013C32012);863基金项目(No.2011AA100806)资助

摘　　要：建立了超高效液相色谱-串联质谱法（UPLC-MS/MS）测定辣椒和土壤中溴氰虫酰胺及其代谢物（J9Z38）残留量的方法,研究了溴氰虫酰胺和J9Z38在辣椒和土壤上的降解特性。样品经乙腈提取后用C18固相萃取柱净化,采用梯度洗脱程序、BEH C18色谱分离柱、应用UPLC-MS/MS正离子扫描测定溴氰虫酰胺和J9Z38。进行了添加浓度为0.01、0.10和1.00 mg/kg的回收实验,溴氰虫酰胺和J9Z38在辣椒和土壤中的日内平均回收率为88.6%~105.7%,日内相对标准偏差为3.8%~15.1%;日间平均回收率为91.4%~105.3%,日间相对标准偏差为4.9%~12.3%。溴氰虫酰胺和J9Z38在2.0~128.0μg/L浓度范围内相关系数r〉0.9992,定量限分别为0.1和0.2μg/kg。应用本方法检测了田间实验样品,结果表明,溴氰虫酰胺在辣椒和土壤中降解半衰期分别为9.2~11.2 d和9.2~20.8 d,J9Z38在辣椒中残留量低于定量限,在土壤中降解半衰期为9.4 d;随着降水量增加,溴氰虫酰胺降解速度加快。An analytical method based on ultra performance liquid chromatography-tandem mass spectrometry was developed for the determination of cyantraniliprole and its main metabolite J9 Z38 residues in pepper and soil. The fate of cyantraniliprole and J9Z38 in pepper and soil was also evaluated. The target compounds were extracted with acetonitrile, cleaned up by C18 cartridge, and further analyzed by gradient ultra performance liquid chromatography-tandem mass spectrometry with electrospray ionization in positive mode （ ESI﹢） using a UPLC BEH C18 Column. The method was validated using fortified pepper and soil. Intra-day mean recoveries of cyantraniliprole and J9Z38 at three spiked levels （0. 01, 0. 10 and 1. 00 mg/kg） ranged from 88. 6% to 105 . 7% with relative standard deviations of 3 . 8%-15 . 1%. Inter-day mean recoveries of cyantraniliprole and J9 Z38 were found between 91 . 4% and 105 . 3% with relative standard deviations of 4 . 9%-12 . 3% at three spiked levels. Limits of quantification （ LOQs） of cyantraniliprole and J9Z38 were 0. 1 and 0. 2 μg/kg, respectively. Linear calibration functions with correlation coefficients of r〉0. 9992 were obtained in the concentration range of 2. 0-128. 0 μg/L. This method was applied to the analysis of cyantraniliprole and J9Z38 residues in real pepper and soil samples selected from field. The results of the residue dynamic experiment showed that the half-life of cyantraniliprole ranged from 9 . 2 to 11 . 2 days in pepper and from 9 . 2 to 20. 8 days in soil. While, the residues of J9Z38 in pepper were below LOQ, and the half-life of J9Z38 in soil was 9. 4 days. The degradation speed of cyantraniliprole increased with the increase of the precipitation.

关 键 词：溴氰虫酰胺 J9Z38 辣椒 残留 液相色谱-串联质谱 

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