摘要
基于QuEChERS前处理技术,采用气相色谱-三重四极杆串联质谱法建立了柑橘中硝虫硫磷残留量的分析测定方法。样品使用乙腈溶剂提取,QuEChERS前处理净化,基质配标曲线,内标法定量,用色谱柱DB-1701进行分离。通过对质谱参数进行优化,确定硝虫硫磷的定量离子对、定性离子对以及碰撞能。结果表明,在10~500μg/L范围内硝虫硫磷质量浓度与其相应的响应值之间呈现良好的线性关系,相关系数0.9995,平均回收率107.2%~114.3%,相对标准偏差(RSDs,n=7)为3.4%~7.1%,检出限为0.00306 mg/kg,定量限为0.00917 mg/kg。硝虫硫磷在柑橘基质中表现为强基质效应,基质效应为79.3%。说明该方法灵敏、准确、稳定、检测成本较低,可用于柑橘中硝虫硫磷残留量的监测。
An analytical method for determining the residue of xiaochongliulin in citrus was established based on QuEChERS sample preparation and gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS).The samples were extracted using acetonitrile,purified via the QuEChERS,and quantified using the internal standard method with matrix-matched calibration curves.Separation was achieved using a DB-1701 chromatographic column.By optimizing the mass spectrometric parameters,the quantitative ion pair,qualitative ion pairs,and collision energy for xiaochongliulin were determined.The results indicated that within the range of 10–500μg/L,the mass concentration of xiaochongliulin showed a good linear relationship with its corresponding response value,with a correlation coefficient of 0.9995.The average recovery rates ranged from 107.2%to 114.3%,with relative standard deviations(RSDs,n=7)of 3.4%–7.1%.The limit of detection was 0.00306 mg/kg,and the limit of quantification was 0.00917 mg/kg.Xiaochongliulin exhibited a strong matrix effect in the citrus matrix,with a matrix effect value of 79.3%.This method is sensitive,accurate,stable,and cost-effective,making it suitable for monitoring xiaochongliulin residues in citrus.
作者
李映梅
周燕平
环会容
LI Yingmei;ZHOU Yanping;HUAN Huirong(Xiangyun Inspection and Testing Institute,Xiangyun 672100,Yunnan,China;Xiangyun Agricultural Environmental Protection Monitoring Station,Xiangyun 672100,Yunnan,China)
出处
《世界农药》
2025年第12期57-62,共6页
World Pesticide
基金
云南省创新引导与科技型企业培育计划-乡村振兴科技专项-服务型科技特派员(No:202304BK090123)。
