| 固相萃取-超高效液相色谱-串联质谱法测定土壤中咪唑乙烟酸的残留量 |
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| 引用本文： | 张昌朋,刘新刚,徐军,董丰收,郑永权.固相萃取-超高效液相色谱-串联质谱法测定土壤中咪唑乙烟酸的残留量[J].农业环境保护,2010(10):2041-2044. |
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| 作者姓名： | 张昌朋 刘新刚 徐军 董丰收 郑永权 |
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| 作者单位： | 农业部农药化学与应用重点开放实验室 中国农业科学院植物保护研究所,北京100193 |
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| 基金项目： | 中国农业科学院植物保护研究所中央级公益性科研院所基本科研业务费专项资金（2010YW12）; 农业部“农药化学与应用”重点开放实验室开放课题（MOAPCA200909） |
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| 摘 要： | 采用固相萃取（SPE）为样品前处理方法,建立了超高效液相色谱-串联四极杆质谱联用（UPLC-MS/MS）检测土壤中咪唑乙烟酸的残留分析方法。土壤样品经0.1 mol.L-1的氯化铵与氨水缓冲液（pH=10）超声提取、C18SPE柱净化后,应用超高效液相色谱串联四级杆质谱仪多离子反应监测（MRM）定量检测,分别以碎片离子m/z 290〉176和m/z 290〉245进行外标法定量。结果表明,在0.01~0.5mg.kg-1添加水平范围内咪唑乙烟酸的平均添加回收率在83.47%~101.70%之间;相对标准偏差在4.15%~5.28%之间;咪唑乙烟酸的定量检出限（LOQ）为0.075μg.kg-1。该方法灵敏度高,操作简单,定量准确,可用于土壤中咪唑乙烟酸的残留分析。
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| 关 键 词： | 超高效液相色谱-串联质谱 固相萃取 咪唑乙烟酸 土壤 |
Determination of Imazethapyr Residues in Soil Using SPE and UPLC-MS/MS |
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| ZHANG Chang-peng,LIU Xin-gang,XU Jun,DONG Feng-shou,ZHENG Yong-quan.Determination of Imazethapyr Residues in Soil Using SPE and UPLC-MS/MS[J].Agro-Environmental Protection,2010(10):2041-2044. |
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| Authors: | ZHANG Chang-peng LIU Xin-gang XU Jun DONG Feng-shou ZHENG Yong-quan |
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| Institution: | (Key Laboratory of Pesticide Chemistry and Application,Ministry of Agriculture,Institute of Plant Protection,Chinese Academy of Agricul-tural Sciences,Beijing 100193,China) |
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| Abstract: | A method for the determination of imazethapyr residues in soil was estimated based on solid phase extraction and ultra-perfor-mance liquid chromatography-mass spectrometry（UPLC-MS/MS）.The samples were extracted with 0.1 mol.L-1 NH4Cl/NH3.H2O（pH=10） buffer by ultrasonic wave,and cleaned up by C18 SPE cartridge.The imazethapyr residues were analyzed by UPLC-MS/MS under multiple-reaction monitoring mode.The qualitative results were obtained based on retention time,the precursor ion and two daughter ions（m/z 290 176 ion and m/z 290245 ion）,and the quantitative results were on the intention of the characteristic m/z 290176 ion.Average recoveries of imazethapyr in soil samples were found in the range of 83.47%~101.70% at three spiking levels from 0.01 mg.kg-1 to 0.5 mg.kg-1 with rela-tive standard deviations of 4.15%~5.28%.Limit of quantification of imazethapyr was 0.075 μg.kg-1.The method is simple and suitable for the routine and confirmation analysis. |
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| Keywords: | UPLC-MS/MS SPE imazethapyr soil |
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