高效液相色谱-质谱/质谱法测定人参中精甲霜灵的残留量  

Residual Detection of Metalaxyl-M in Ginseng by High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：吕雁斌[1] 王燕[1] 王睿[1] 卢宝慧[1] 杨丽娜[1] 朴承熙 高洁[1] 

机构地区：[1]吉林农业大学农学院,长春130118 [2]集安人参研究所,吉林集安134200

出　　处：《农药》2016年第5期370-373,共4页Agrochemicals

基　　金：吉林省现代农业技术体系建设课题--人参新农药筛选及农药安全使用技术集成与示范(2015024);公益行业(农业)科研专项--人参产业技术研究与示范(201303111)

摘　　要：[目的]建立高效液相色谱-质谱/质谱法测定人参中精甲霜灵残留量的分析方法。[方法]采用外标法定量。检测条件如下:采用N-丙基乙二胺固相萃取柱(PSA),以0.1%甲酸水-乙腈为流动相梯度洗脱,提取时间为5 min,提取溶剂为丙酮,洗脱液为乙腈-甲苯混合溶液(体积比3∶1)。[结果]在选定的色谱质谱条件下,精甲霜灵的最低检出质量分数为0.002 mg/kg;方法的精密度为5.63%～15.62%;准确度为78.0%～89.1%。[结论]该方法符合农药残留检测技术的要求,适用于人参中精甲霜灵残留量的测定。[Aims] The aims were to establish a method for the detection ofmetalaxyl-M in ginseng with HPLC-MS/MS. [Methods] Based on external standard method, the detection conditions were as follows： N-propyl ethylenediamine solid-phase extraction column （PSA）, with 0.1% formic acid-water and acetonitrile as mobile phase and gradient elution. Extraction time was 5 min, acetone as extraction solvent, acetonitrile-toluene （3：1, by vol） as extraction solvent. [Results] Under the optimized chromatography and mass spectra conditions, the limit of detection of metalaxyl-M was 0.002 mg/kg. The precision of this method was 5.63-15.62%, and the accuracy was 78.0-89.1%. [Gonclusions] This method satisfy to the requirements of residue detection and is suitable for metalaxyl-M residue determination in ginseng.

关 键 词：精甲霜灵 高效液相色谱串联质谱 人参 残留 

分 类 号：O657.63[理学—分析化学] TS207.53[理学—化学]