超高效液相色谱-串联质谱法测定辣椒及其栽培土壤中烯酰吗啉和唑嘧菌胺

Determination of dimethomorph and ametoctradin in pepper and soil by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  烯酰吗啉  唑嘧菌胺  超高液相色谱-串联质谱法  辣椒  土壤

英文关键词:dimethomorph  ametoctradin  ultra performance liquid chromatography-tandem mass spectrometry  pepper  soil

中文摘要:

      目的 建立用于辣椒和土壤中烯酰吗啉和唑嘧菌胺残留检测的超高效液相色谱-串联质谱方法。方法 辣椒和土壤样品采用乙腈和水提取, 盐析后取上清液, 通过优化色谱分离等条件, 建立超高效液相色谱-串联质谱方法, 结合目标物标准曲线进行定量分析。结果 经过3个水平的加标回收率实验, 所建立方法的平均回收率在85.2%～97.8%, 相对标准偏差0.1%～2.2%(n=5)。烯酰吗啉在辣椒的定量限为0.04 mg/kg, 在土壤中定量限为0.01 mg/kg; 唑嘧菌胺在辣椒和土壤中的定量限均为0.01 mg/kg。结论 所建立的分析方法操作简便, 分离净化效果良好, 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 dimethomorph and ametoctradin residuals in pepper and soil by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Method Pepper and soil samples were extracted by mixture of acetonitrile and water, and supernatant was analyzed through UPLC-MS/MS after salted out. Quantitative analysis was carried out with the standard curve of the target pesticides. Results According to the results of 3 levels of spiked recovery experiments, the average recoveries of the established method ranged from 85.2% to 97.8%, and the relative standard deviations (RSDs) ranged from 0.1% to 2.2% (n=5). The limits of quantitation (LOQs) of dimethomorph in pepper and soil were respectively 0.04 mg/kg and 0.01 mg/kg, and LOQs of ametoctradin in pepper and soil were both 0.01 mg/kg. Conclusion The established method is simple and convenient, and the separation and purification effects are good. The sensitivity, accuracy and precision of the established method can match the requirements of pesticide residue detection.