UPLC-MS/MS快速测定烟草中2,4-滴和2,4,5-涕

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为测定烟草中2种常见的氯代苯氧羧酸类除草剂残留,通过对实验条件的优化,建立了一种测定烟草中2,4-滴和2,4,5-涕的超高效液相色谱-串联质谱(UPLC-MS/MS)方法.样品经盐酸水溶液和CH2Cl2萃取净化后,用C18色谱柱分离,在多反应离子监测模式(MRM)下进行定性与定量分析.结果表明:①2,4-滴和2,4,5-涕在对应标准工作曲线范围内线性关系良好(r>0.999),检出限(LOD)和定量限(LOQ)分别为 0.004 5~0.007 6 和 0.013 8~0.023 6 mg/kg,回收率为 79.5%~94.6% ,相对标准偏差(RSDs)<6.0%.②采用该方法对30个不同类型的烟草样品进行了检测,检测结果与烟草行业标准方法检测结果无明显差异.该方法无需衍生化,具有分析速度快、灵敏度高、溶剂消耗少等优点,适用于烤烟、白肋烟和香料烟中2,4-滴和2,4,5-涕的定量分析.“,”In order to analyze two common chlorinated phenoxy acid residues in tobacco, an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for quantifying 2,4-D and 2,4,5-T was proposed. The analytes were extracted from tobacco samples by a hydrochloric acid solution and CH2Cl2. The extract was analyzed qualitatively and quantitatively by a tandem mass spectrometer in multiple reaction monitoring (MRM) mode after being separated on C18 column. The results showed that: 1) A good linear relation was obtained in the range of standard working solution with r>0.999. The limits of detection (LODs) and quantification (LOQs) were 0.004 5-0.007 6 and 0.013 8-0.023 6 mg/kg, respectively. The added standard recoveries of blank samples ranged from 79.5% to 94.6% with the relative standard deviations less than 6.0% . 2) The method was applied to 30 different types of tobacco samples, the results agreed well with those obtained by the tobacco industry standard method based on GC-MS. The proposed method is rapid and sensitive, no derivatization required, and consumes less organic reagents. It is suitable for the analysis of 2,4-D and 2,4,5-T in flue-cured tobacco, burley tobacco and oriental tobacco.
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