测定葡萄中苯醚甲环唑、己唑醇和咪鲜胺代谢物残留量方法研究

Determination of difenoconazole, hexaconazole and prochloraz metabolite residues in grapes

中文关键词:  苯醚甲环唑  己唑醇  咪鲜胺  2,4,6-三氯苯酚  葡萄

英文关键词:difenoconazole  hexaconazole  prochloraz  2,4,6-trichlorophenol  grapes

中文摘要:

      目的 建立用于葡萄中苯醚甲环唑、己唑醇和咪鲜胺残留检测的分析方法。方法 葡萄样品先经乙腈和水提取, 盐析后取上清液进行水解并测定。通过优化前处理及色谱条件, 建立色谱分析方法, 结合目标物标准曲线进行定量分析。结果 经过3个水平的加标回收实验, 所建立方法的平均回收率在79%~102%, 相对标准偏差0.5%~6.9%(n=5)。苯醚甲环唑和己唑醇的最低检出浓度为0.01 mg/kg, 2,4,6-三氯苯酚的最低检出浓度为0.2 mg/kg。结论 所建立的分析方法操作简便, 分离净化效果良好, 显著提高前处理效率, 灵敏度、准确度和精密度均达到农药残留检测要求。

英文摘要:

      Objective To establish a method for determination of difenoconazole, hexaconazole and prochloraz residues in grapes by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and gas chromatography (GC). Methods Grape samples were extracted by mixture of acetonitrile and water, supernatant was hydrolyzed and analyzed after salted out. UPLC-MS/MS and GC methods were established after optimization of the pretreatments and chromatographic conditions. Quantitative analysis was carried out with the standard curve of the target pesticides. Results According to the results of a 3 level standard recovery experiment, the average recoveries of the established method ranged from 79% to 102%, and the relative standard deviations (RSDs) ranged from 0.5% to 6.9% (n=5). The limits of quantitation (LOQs) of difenoconazole and hexaconazole in grapes were 0.01 mg/kg, while the LOQ of prochloraz was 0.2 mg/kg. Conclusion The established analytical method is simple to operate, has good separation and purification effect, significantly improves the pretreatment efficiency, and meets the requirements of pesticide residue detection with sensitivity, accuracy and precision.