苹果叶片中吡唑醚菌酯残留的超高效液相色谱-串联质谱检测方法

发布时间：2018-06-18 02:06

本文选题：苹果 + 叶片　；参考：《农药学学报》2016年06期

【摘要】：为了解吡唑醚菌酯在苹果叶片中的残留动态,合理评估其持效期,比较了液液萃取、固相萃取以及Qu ECh ERS(Quick、Easy、Cheap、Effective、Rugged、safe)3种样品前处理方法对苹果叶片中吡唑醚菌酯添加回收率的影响,优化了基于超高效液相色谱-串联质谱(UPLCMS/MS)的检测条件与方法。结果表明:采用Qu ECh ERS法提取时回收率较高,所需有机溶剂少,时间短,重复性好,适合苹果叶片中吡唑醚菌酯的萃取和净化;对于苹果叶片,萃取和净化步骤中的填料可减少为乙二胺-N-丙基甲硅烷(PSA)和石墨化碳黑(GCB)2种,其最佳用量PSA为0.025 g/m L,GCB为0.020 g/m L;苹果叶组织对样品检测具有微弱的基质增强效应。通过对Qu ECh ERS方法的改进以及对色谱-质谱检测参数的优化,建立了苹果叶片中吡唑醚菌酯残留的检测方法,该方法的线性范围为0.01~50.0 mg/L,定量限为0.01 mg/kg。在0.01~10 mg/kg4个添加水平下,吡唑醚菌酯在苹果叶片中的回收率为92%~99%,相对标准偏差为2.2%~5.3%。田间实测结果表明:苹果叶片喷施1 000 mg/L的25%吡唑醚菌酯乳油,其残留消解动态符合一级反应动力学模型c_t=79.87 e~( 0.053 3 t),半衰期为13 d。
[Abstract]:In order to understand the residual dynamics of pyrazole in apple leaves and evaluate its retention period reasonably, the effects of liquid-liquid extraction, solid phase extraction and QUECH ERSX QY EasyEY Effective Effective RuggedSafeto on the recovery of pyrazole in apple leaves were compared. The detection conditions and methods based on ultra high performance liquid chromatography-tandem mass spectrometry (UPLCs / MS) were optimized. The results show that the recovery rate is high, the organic solvent is less, the time is short and the repeatability is good, which is suitable for the extraction and purification of pyrazole in apple leaves. In the extraction and purification process, the fillers can be reduced to ethylenediamine-N-propylmethylsilane (PSAs) and graphitized carbon black (GCBs), the optimum dosage of which is 0.025 g / m ~ (-1) GCB = 0.020 g / m ~ (L), and apple leaf has a weak matrix enhancement effect on sample detection. By improving the QU ECh ERS method and optimizing the detection parameters of the chromatography-mass spectrometry, a method for the determination of pyrazolyl ester residues in apple leaves was established. The linear range of the method was 0.01 ~ 50.0 mg / L, and the quantitative limit was 0.01 mg / kg 路L ~ (-1). The recovery rate of pyrazole in apple leaves was 92 and the relative standard deviation was 2.2 / 5.3under the addition level of 0.01 ~ 10 mg/kg4. The field test results showed that the residual digestion kinetics of apple leaves sprayed with 25% Pyrazolyl Ester EC of 1 000 mg / L was consistent with the first-order reaction kinetics model c_t=79.87 (0.053 3 t ~ (-1) with a half-life of 13 days.
【作者单位】：青岛农业大学农学与植物保护学院/山东省植物病虫害综合防控重点实验室;
【基金】：现代农业产业技术体系(CARS-28) 山东省泰山学者建设工程专项资助经费
【分类号】：S481.8;O657.63

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