高通量全自动仪器法测定植物源性食品中甲基托布津残留量

High-throughput Automated Instrumental Analysis of Thiophanate-methyl Residue in Plant-derived Foods

建立高效的应用高通量全自动均质仪、全自动净化在线浓缩仪及液相色谱-串联质谱仪测定植物源性食品中甲基托布津残留量的检测方法。试样经高通量全自动均质仪,用乙腈均质提取,经全自动净化在线浓缩仪(凝胶色谱柱、固相萃取柱)净化、在线浓缩后,采用液相色谱-串联质谱仪定量定性分析,外标法定量,液相流动相为甲醇-水,采用电喷雾离子源,定性离子对为m/z 343.0>151.1、m/z 343.0>192.1,定量离子对为m/z 343.0>151,添加0.01～10.0mg/kg的甲基托布津标准品时的回收率为88.4%～97.9%,相对标准偏差(RSD)在1.3%～2.9%之间,最低检出限为0.01mg/kg。该方法特异性强、敏感性高、高通量、全自动、快速高效,可应用于植物源性食品的甲基托布津残留量检测。

An efficient detection method for thiophanate methyl residue in plant-derived foods was established by combing a high-throughput automated homogenizer,an automatic online purification and concentration system and a liquid chromatog-raphy-tandem mass spectrometry.Samples were homogenized with acetonitrile on a high-throughput automated homogenizer,purified using an automatic online purification（gel chromatographic and solid phase extraction column） system,online concen-trated and detected using a liquid chromatography-tandem mass spectrometer.The quantification of thiophanate methyl was carried out using the external standard method.The detection conditions were： acetonitrile-water（gradient） as mobile phase,ESI as ionization method,qualitative ion pairs of m/z 343.0 151.1 and 343.0 192.1,quantitative ion pairs of m/z 343.0 151.1.With the addition of 0.01 to 10.0 mg/kg of thiophanate standard to samples,the recovery rate was between 88.4% and 97.9% and the relative standard deviations（RSDs） varied from 1.3% to 2.9%.The detection limit of the established method was 0.01 mg/kg.