PTV-GC-MS/MS同时测定烟草中202种农药残留
Simultaneous Determination of 202 Pesticide Residues in Tobacco by PTV-Gas ChromatographyTandem Mass Spectrometry
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摘要: 研究了应用程序升温汽化进样-气相色谱-串联质谱(PTV-GC-MS/MS)技术检测烟草中202种农药品种221个组分的高效方法。以QuEChERS技术快速提取烟草中残留农药并净化,PTV进样后在TR-pesticide Ⅱ毛细管柱上分离,通过优化串联质谱参数,有效降低复杂基质干扰及农药组分重叠峰的相互串扰,以保留时间窗口和特征SRM(选择性反应监测)离子对定性、峰面积定量。结果表明:①202种农药在0.01~2.50 mg/L范围内线性良好,相关系数为0.9800~0.9999,检测限0.0002~0.0100 mg/kg,加标回收率67.4%~112.0%,RSD 0.30%~20.30%。②应用该方法对44个进口烟叶样品进行检测验证,效果良好。③该方法对农药品种覆盖面广,前处理简便、快捷,节省溶剂;一次进样在46 min内可分析221个组分,准确、灵敏。Abstract: An effective method for detecting 202 pesticide residues (221 components) in tobacco was developed by PTV-GC-MS/MS (Programmed temperature vaporization sampling technology-gas chromatography-tandem mass spectrometry). The pesticide residues in tobacco sample were extracted rapidly and purified with QuEChERS technique, then separated on TR-pesticideⅡ capillary chromatographic column after PTV sampling. The interference of complex matrix and peak overlapping of various pesticide components were reduced by means of optimizing tandem mass spectrometry parameters. Qualitative and quantitative analyses were conducted by retention time window and SRM (selective reaction monitoring) with peak area respectively. The results showed that:1) The 202 pesticides kept good linear relationships in the range of 0.01-2.50 mg/L with the correlative coefficients between 0.9800 and 0.9999. The limits of detection (LOD) were from 0.0002 to 0.0100 mg/kg, and the recoveries of added standards ranged from 67.4% to 112.0% with the relative standard deviations (RSD) of 0.30%-20.30%. 2) This method was verified with 44 samples of imported tobacco leaves, and results were satisfied. 3) This method covered a wide range of pesticides, featured the advantages of simple and rapid in pre-treatment, solvent saving and capable of analyzing 221 components accurately and sensitively within 46 minutes by a single sample injection.
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