QuEChERS-超高效液相色谱-串联质谱法测定玉米植株和土壤中溴氰虫酰胺及其代谢物残留

Determination of cyantraniliprole and its metabolite in maize plant and soil by QuEChERS and ultra-performance liquid chromatography tandem mass spectrometry

建立了超高效液相色谱-串联质谱（UPLC-MS/MS）测定玉米植株和土壤中溴氰虫酰胺及其代谢物J9Z38残留量的方法,明确了种子处理方式下两种化合物的消解动力学。样品经乙腈提取,采用QuEChERS方法处理后,进UPLC-MS/MS检测分析。结果表明：在0.01、0.1和1 mg/kg添加水平下,溴氰虫酰胺和J9Z38在玉米植株和土壤中的平均回收率在81%～103%之间,相对标准偏差均小于10.1%;在0.1～50μg/L范围内,溴氰虫酰胺和J9Z38的质量浓度与相应峰面积间线性关系良好（R2〉0.999）,定量限（LOQ）均为0.01 mg/kg。溴氰虫酰胺和J9Z38在玉米植株和土壤中的消解动态符合一级动力学模型,溴氰虫酰胺在玉米植株和土壤中的消解半衰期分别为8.3和8.2 d（春季）,3.9和4.5 d（夏季）。该方法简单、灵敏、高效,能够满足溴氰虫酰胺及其代谢物J9Z38在玉米植株和土壤中残留的检测需求。

An efficient method for the determination of cyantraniliprole and its metabolite J9Z38 residues in maize plant and soil were established using ultra-performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS）. The fate of cyantraniliprole and J9Z38 in maize plant and soil after seed treatment was also evaluated. The target compounds were extracted with acetonitrile,pretreated using QuEChERS method and analyzed by UPLC-MS/MS. The mean recoveries of cyantraniliprole and J9Z38 at three spiked levels（0.01, 0.1 and 1 mg/kg） ranged from 81% to 103%,respectively, with relative standard deviations both less than 10.1%. The results demonstrate the concentrations of cyantraniliprole and J9Z38 have a good linear relationship with the corresponding peak area in the range of 0.1-50 μg/L, with dertermination coefficient（R^2 0.999）, and limits of quantitation were 0.01 mg/kg. The dissipation dynamics of cyantraniliprole and J9Z38 were both in line with the first order kinetic equation. The half-lives of cyantraniliprole in maize plant and soil were 8.3 and 8.2 d（in spring）, and 3.9 and 4.5 d（in summer）, respectively. All the above observations indicate that the established analytical method is sample, sensitive, highly efficient, and suitable for monitoring the residues of cyantraniliprole and its metabolite J9Z38 in maize plant and soil.