HPLC-MS/MS测定不同基质中啶酰菌胺和多杀霉素残留量  

Determination of Boscalid and Spinosad Residues in Different Matrixs by HPLC-MS/MS

作　　者：王思威[1] 刘艳萍[1] 孙海滨[1] 

机构地区：[1]广东省农业科学院植物保护研究所广东省植物保护新技术重点试验室,广州510640

出　　处：《农药》2017年第12期897-900,共4页Agrochemicals

基　　金：广东省农业科学院院长基金(201707)

摘　　要：[目的]建立一种苹果、香蕉和柑橘中啶酰菌胺和多杀霉素的高效液相色谱-串联质谱(HPLC-MS/MS)快速检测分析方法。[方法]样品采用乙腈作为提取溶剂、氨基固相萃取小柱为净化柱,高效液相色谱串联质谱仪正离子扫描模式检测不同基质中啶酰菌胺和多杀霉素残留量。[结果]啶酰菌胺和多杀霉素在苹果、香蕉和柑橘不同基质中平均添加回收率分别为83.96%~109.78%、83.49%~99.38%,相对标准偏差分别为3.38%~13.17%、1.99%~7.98%;定量限LOQ均为0.01 mg/kg,检出限LOD均为0.005 mg/L。[结论]前处理方法简洁快速、净化效果好,高效液相色谱串联质谱仪的定性和基质标溶液定量分析方法精准,准确度、精密度等均符合农药残留检测分析要求。[Aims] The aim was to establish the method for determination of boscalid and spinosad residues in apple,banana and citrus by SPE and high performance liquid chromatography tandem-mass spectrometry（HPLC-MS/MS）.[Methods] The samples were extracted with acetonitrile, cleaned-up by the column of NH2-SPE, and detected by HPLC-MS/MS. [Results] The average recoveries of boscalid ranged from 83.96 to 109.78% with the relative standard deviation（RSD） of 3.38-13.17%, the average recoveries of spinosad in apple, banana and citrus were 83.49-99.38%with the RSD of 1.99-7.98%. The limit of quantitation（LOQ） and limit of detection（LOD） was 0.01 mg/kg and 0.005 mg/L,respectively. [Conclusions] This method is quick, convenient, less time and organic solvents. The accuracy and precision could meet the requirements for pesticide residue detection, which is suitable for analysis of boscalid and spinosad residues in different matrixs.

关 键 词：啶酰菌胺 多杀霉素 高效液相色谱-串联质谱 农药残留 

分 类 号：O657.63[理学—分析化学] TQ450.263[理学—化学]