高效液相色谱-串联质谱法测定水果中7种苯甲酰脲类杀虫药的残留量  

Rapid HPLC-MS/MS Determination of Residual Amounts of 7 Benzoylurea Insecticides in Fruits

作　　者：艾连峰[1] 王凤池[1] 陈瑞春[1] 郭春海[1] 李玮[1] 

机构地区：[1]河北出入境检验检疫局,石家庄050051

出　　处：《理化检验（化学分册）》2010年第9期989-992,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出了高效液相色谱-串联质谱法测定水果中7种苯甲酰脲类杀虫药（除虫脲、灭幼脲、杀铃脲、氟铃脲、氟苯脲、氟虫脲和氟啶脲）残留量的方法。该方法采用多反应监测（MRM）负离子扫描模式,可一次对水果中7种苯甲酰脲类杀虫药进行准确的定性和定量分析;样品用石油醚提取,提取液经分取、水浴45℃氮气吹干、溶解后进行分析。除虫脲、灭幼脲、杀铃脲、氟虫脲和氟啶脲的测定下限（10S/N）为2μg·kg^-1,氟铃脲和氟苯脲测定下限（10S/N）为0.5μg·kg^-1。7种苯甲酰脲类杀虫药在100-内呈线性。方法在3个水平的加标回收率在83.8%-94.4%之间,日内相对标准偏差在3.12%-7.43%之间,日间相对标准偏差在3.96%-7.63%之间。Residual amounts of 7 benzoylurea insecticides,i.e.,diflubenzuron,chlorbenzuron,triflumuron,hexaflumuron,flubenzuron,flufenozuron and chlorfluazuron,were determined by HPLC-MS/MS.The mode of multi-reaction monitoring negative ion scanning was adopted for both the quantitative and qualitative analysis.The fruit sample was extracted with petroleum ether,an aliquot of the extract was taken and evaporated to dryness by blowing with nitrogen when heated in a water bath at 45 ℃.The residue was taken up with 1.0 mL of methanol and used for HPLC-MS/MS analysis.The values of lower limit of determination（10S/N） of 2 μg·kg^-1ere found for each of diflubenzuron chlorbenzuron,triflumuron,flufenoxuron and chlorfluazuron,and of 0.5 μg·kg^-1or hexaflumuron and flubenzuron.Linear relationships in the range within 100 μg·kg^-1ere found for all of the 7 insecticides.Recovery and precision of the method were tested by standard addition method at 3 concentration levels.Results obtained were as follows： recovery 83.8%-94.4%;RSD′s（n=9） of repeatability 3.12%-7.43%,RSD′s（n=9） of reproducibility 3.96%-7.63%.

关 键 词：高效液相色谱-串联质谱法 苯甲酰脲类农药 残留量 水果 

分 类 号：O657.63[理学—分析化学]