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%.
An 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 externa/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%.
出处
《分析测试技术与仪器》
CAS
2012年第4期204-207,共4页
Analysis and Testing Technology and Instruments
基金
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)
国家质检总局科技计划项目(2012IK160)
