农药学学报2016，Vol.18Issue(6)：752-758,7.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 inMalus domestica leaves
摘要
Abstract
A new method was developed for the residue determination of pyraclostrobin inMalus 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 equationct=79.87 e–0.053 3t, and the half-life period (DT50) was 13 days according to this model.关键词
苹果/叶片/吡唑醚菌酯/残留/QuEChERS法/超高效液相色谱-串联质谱Key words
Malus domestica/leaves/pyraclostrobin/residue/QuEChERS/UPLC-MS/MS分类
农业科技引用本文复制引用
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):752-758,7.基金项目
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 （CARS-28）
