荔枝中抑霉唑和嘧霉胺残留量的超高效液相色谱-串联质谱法同时测定  

Simultaneous Determination of Residues of Imazalil and Pyrimethanil in Litchi by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：王玉健[1] 黄惠玲[1] 汪春光[1] 蔡伟凯 刘红专[1] 卓海华[1] 

机构地区：[1]海南出入境检验检疫局技术中心,海南海口570311

出　　处：《分析测试学报》2010年第10期1068-1072,共5页Journal of Instrumental Analysis

摘　　要：建立了超高效液相色谱-串联质谱法同时测定荔枝中抑霉唑和嘧霉胺的方法,对提取试剂、流动相、质谱条件进行了研究,并对抑霉唑和嘧霉胺可能的断裂机理进行了推测。待测样品直接用乙腈提取,采用电喷雾离子源(ESI)、多反应监测正离子模式扫描,外标法定量。抑霉唑、嘧霉胺的质量浓度在1.00～20.0μg/L范围内与峰面积呈良好线性,方法的检出限为0.005mg/kg;添加水平为0.005、0.010、0.020mg/kg时抑霉唑和嘧霉胺的平均回收率分别为91%～96%和83%～90%,相对标准偏差分别为6.5%～8.4%和9.5%～11.1%。该方法快速、简便、准确,可用于荔枝中抑霉唑和嘧霉胺残留量的定性与定量检测。An ultra performance liquid chromatography tandem mass spectrometric method was established for the simultaneous determination of residues of imazalil and pyrimethanil in litchi sample.The effects of extration condition,flow phase,and tandem mass spectrometric parameters were investigated.The possible fragmentation mechanisms of imazalil and pyrimethanil were discussed.The sample was extracted with acetonitrile.The analysis on analytes was carried out under the multiple reaction monitoring（MRM）mode by employing the external method.The calibration curves of imazalil and pyrimethanil were linear in the range of 1.00-20.0 μg/L.The limits of detection（LOD）were both 0.005 mg/kg.The average recoveries of imazalil and pyrimethanil at spiked levels of 0.005,0.010,0.020 mg/kg were in the range of 91%-96% and 83%-90%,respectively,and their relative standard deviations（RSDs）were 6.5%-8.4% and 9.5%-11.1%,respectively.The method was fast,convenient,accurate,and could be used as a reliable means for the simultaneous quantitative determination of residues of imazalil and pyrimethanil in litchi sample.

关 键 词：抑霉唑 嘧霉胺 荔枝 超高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学] S767.1[理学—化学]