王玉然, 梁化雨, 李平亮, 李保华. 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[J]. 农药学学报, 2016, 18(6): 752-758. DOI: 10.16801/j.issn.1008-7303.2016.0106
    引用本文: 王玉然, 梁化雨, 李平亮, 李保华. 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[J]. 农药学学报, 2016, 18(6): 752-758. DOI: 10.16801/j.issn.1008-7303.2016.0106
    WANG Yuran, LIANG Huayu, LI Pingliang, LI Baohua. Development and validation of an ultra-performance liquid chromatography-tandem mass spectrometry method for the residue analysis of pyraclostrobin in Malus domestica leaves[J]. Chinese Journal of Pesticide Science, 2016, 18(6): 752-758. DOI: 10.16801/j.issn.1008-7303.2016.0106
    Citation: WANG Yuran, LIANG Huayu, LI Pingliang, LI Baohua. Development and validation of an ultra-performance liquid chromatography-tandem mass spectrometry method for the residue analysis of pyraclostrobin in Malus domestica leaves[J]. Chinese Journal of Pesticide Science, 2016, 18(6): 752-758. DOI: 10.16801/j.issn.1008-7303.2016.0106

    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

    Development and validation of an ultra-performance liquid chromatography-tandem mass spectrometry method for the residue analysis of pyraclostrobin in Malus domestica leaves

    • 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QuEChERS(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QuEChERS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/mL,GCB为0.020 g/mL;苹果叶组织对样品检测具有微弱的基质增强效应。通过对QuEChERS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9 2%~9 9%,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ct=79.87 e-0.053 3 t,半衰期为13 d。

       

      Abstract: A new method was developed for the residue determination of pyraclostrobin in Malus domestica leaves. The recovery rates of pyraclostrobin with three pretreatment methods were investigated and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was employed for the analysis. Results showed that Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) had a better recovery, required less solvent and shorter time. In the purification procedure of QuEChERS, only two substances, PSA and GCB, were added. Good extracting and purification results can be obtained by using PSA and GCB with the dosages of 0.025 and 0.020 mg/mL respectively. Apple leaf tissues had slight enhancement matrix effect in the residue analysis of pyraclostrobin. In this work, a method for the residue analysis of pyraclostrobin in apple leaves was developed by using the improved QuEChERS method and the UPLC-MS/MS instrument. Following the proposed method, the linearity was in the range of 0.01-50.0 mg/L with the quantitation limit (LOQ) of 0.01 mg/kg and the recovery ranged between 92% and 99% with the RSD range of 2.2%-5.3%. The proposed method was applied to study the residue dynamic of pyraclostrobin in apple leaves. The detected data of pyraclostrobin residue in apple leaves can be well described by the first order kinetics equation ct=79.87 e-0.053 3 t, and the half-life period (DT50) was 13 days according to this model.

       

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