颜鸿飞, 李拥军, 王美玲, 戴华, 张莹, 黄志强. 高效液相色谱-串联质谱法测定水果中残留的烯唑醇[J]. 分析测试技术与仪器, 2012, 18(4): 204-207.
引用本文: 颜鸿飞, 李拥军, 王美玲, 戴华, 张莹, 黄志强. 高效液相色谱-串联质谱法测定水果中残留的烯唑醇[J]. 分析测试技术与仪器, 2012, 18(4): 204-207.
YAN Hong-fei, LI Yong-Jun, WANG Mei-Ling, DAI Hai, ZHANG Ying, HUANG Zhi-Qiang. Determination of Diniconazole Residue in Fruits by HPLC-MS/MS[J]. Analysis and Testing Technology and Instruments, 2012, 18(4): 204-207.
Citation: YAN Hong-fei, LI Yong-Jun, WANG Mei-Ling, DAI Hai, ZHANG Ying, HUANG Zhi-Qiang. Determination of Diniconazole Residue in Fruits by HPLC-MS/MS[J]. Analysis and Testing Technology and Instruments, 2012, 18(4): 204-207.

高效液相色谱-串联质谱法测定水果中残留的烯唑醇

Determination of Diniconazole Residue in Fruits by HPLC-MS/MS

  • 摘要: 建立了水果中烯唑醇残留量的高效液相色谱-串联质谱(LC-MS/MS)测定方法。样品采用丙酮-正己烷液液振荡提取,经分散固相萃取(DSPE)净化后,采用ODS-C18柱为分离柱,以乙腈-0.1%甲酸溶液为流动相,采用液相色谱-串联质谱(ESI)多反应监测(MRM)正离子模式测定,外标法定量。烯唑醇在0.002~0.2 mg//L质量浓度范围内线性关系良好,方法定量下限(LOQ)为0.001 mg/kg。在0.005~0.1 mg/kg之间的3个添加浓度水平下,添加回收率为78.8 %~108.0 %,相对标

     

    Abstract: high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) analytical method for the determination of diniconazole residues in the fruits has been developed. Samples are liquid-liquid extracted with acetone - hexane and clean up with dispersive solid phase extraction (DSPE). The analyte is separated on an ODS-C18 column with acetonitrile-0.1% formic acid solution as the mobile phase.The target compound is detected by LC-MS/MS (ESI +) under the multiple reaction monitoring (MRM) mode using an external standard method. The linear relationship of this method was good between 0.002~0.2 mg/L concentration range. The limit of quantification (LOQ) was 0.001 mg/kg. The recoveries of diniconazole ranged from 78.8% to 108.0% at the three spiked levels of 0.005~0.1 mg/kg and the relative standard deviations(RSDs) were in range of 2.1%~6.9%.

     

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