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高效液相色谱-串联质谱法测定水果中残留的烯唑醇
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.
作者姓名:颜鸿飞  李拥军  王美玲  戴华  张莹  黄志强
作者单位:湖南出入境检验检疫局食品安全科学技术湖南省重点实验室,湖南长沙,410004
基金项目:国家质检总局科研制标项目(2010B385r)、食品安全国家标准项目(spaq-2012-68)和国家质检总局科技计划项目(2012IK160)
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%,相对标准偏差(RSDs)为2.1% ~6.9%.

关 键 词:高效液相色谱-串联质谱  分散固相萃取  烯唑醇  水果
收稿时间:8/5/2012 12:00:00 AM
修稿时间:2012/9/29 0:00:00

Determination of Diniconazole Residue in Fruits by HPLC-MS/MS
YAN Hong-fei,LI Yong-Jun,WANG Mei-Ling,DAI Hai,ZHANG Ying and 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.
Authors:YAN Hong-fei  LI Yong-Jun  WANG Mei-Ling  DAI Hai  ZHANG Ying and HUANG Zhi-Qiang
Institution:(Technology Center Hunan Entry-Exit Inspection and Quarantine Bureau,Food Safety Science and Technology Key laboratory of Hunan Province,Changsha 410004,China)
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%.
Keywords:
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