Evaluation of systemic properties of penflufen in wheat seedling using ultra performance liquid chromatography-tandem mass spectrometry method
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摘要: 建立了超高效液相色谱-串联质谱（UPLC-MS/MS）测定氟唑菌苯胺在小麦植株中内吸传导特性的方法；定量分析了在小麦根部和叶部施药2种处理方式下氟唑菌苯胺进入植株后的分布和累积情况。植株样品前处理采用QuEChERS法，在反相色谱柱C18（100 mm × 2.1 mm， 1.8 μm）上，以0.1%甲酸水和乙腈为流动相，利用梯度洗脱，正离子电离（ESI+），采用多反应离子监测模式（MRM）进行定性和定量。用基质匹配标准溶液外标法定量。结果表明：在0.5~100 μg/L内，氟唑菌苯胺的质量浓度与对应的峰面积间线性关系良好，线性回归方程为y = 12 808.4x + 308.518（r = 0.999 8）。在0.005、0.05和0.1 mg/kg添加水平下，氟唑菌苯胺在小麦植株中的回收率为92%~126%，相对标准偏差为0.50%~9.1%；以3倍信噪比计算，方法检出限为0.037 μg/kg；最低添加浓度为0.005 mg/kg。研究结果表明，氟唑菌苯胺于小麦植株根部施用后，可迅速在根部吸收并向茎部传导，且随处理浓度增大，药剂在不同部位的累积量增加；随处理后时间延长，药剂在不同部位的累积表现为先快速吸收而后缓慢平衡。其中以0.01 mg/L氟唑菌苯胺经根部施药2 h后，药剂在根、茎和叶中含量分别为10.4、0.6和0.3 μg/kg；氟唑菌苯胺经叶部单叶片施药后，亦可快速被叶片吸收，并可跨叶传导至其他叶片，进而在茎部和根部累积。随处理后时间延长，施药叶片药剂快速下降并达到平衡，其他植株部位药剂快速累积并达到平衡。其中以200 mg/L的氟唑菌苯胺经第2片叶施用20 μL，2 h后氟唑菌苯胺在根和茎中的含量分别为109.0和148.0 μg/kg，在第3片叶和旗叶中的含量分别为904.0和112.6 μg/kg。
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关键词:
- 氟唑菌苯胺 /
- 超高效液相色谱-串联质谱 /
- 小麦植株 /
- 内吸传导
Abstract: The transportation and the contents of penflufen accumulated in roots, stems and leaves of wheat seedling were determined by ultra performance liquid chromatography-tandem mass spectrometry method after it was applied to roots or leaves. A QuEChERS method was used for the extraction and clean-up of wheat seedling samples. Chromatographic analysis was performed on an Endeavorsil C18 column (100 mm × 2.1 mm, 1.8 μm) using gradient elution with 0.1% formic acid in water and acetonitrile as mobile phase. Elutes were ionized through positive ion ionization (ESI+) mode. Qualitative and quantitative was conducted by multi reaction ion monitoring (MRM). The external standard method of matrix matching standard solution was used. The good linear relationship was obtained in the range of 0.5-100 μg/L and the equation was y = 12 808.4x + 308.518 (r = 0.999 8). The recovery of penflufen in wheat seedling ranged from 92% to 126%. The relative standard deviation was between 0.50% to 9.1%. The minimum detection limit was 0.037 μg/kg(S/N = 3) and the minimum fortified level was 0.005 mg/kg. The study indicated that penflufen had rapid intake and transportation with root application. With the increase of the treatment concentration, the accumulation of penflufen in different plant parts increased. With the extension of treatment time, the accumulation of penflufen in different parts showed rapid absorption and then slowly balanced. When wheat root was treated by 0.01 mg/L penflufen, its content in root, stem and leaf were 10.4, 0.6 and 0.3 μg/kg, respectively 2 h after treatment. In addition, penflufen was rapidly absorbed by leaves and then transported to other leaves and accumulated at stems and roots with leaves application. With the extension of the treatment time, the pesticide in the leaves decreased rapidly and eventually reached equilibrium, and other plant parts accumulated rapidly and reached equilibrium. When the 2nd leaf of wheat was treated by 20 μL penflufen aqueous solution its contents in root, stem, 3rd leaf and 1st leaf were 109.0, 148.0, 904.0 and 112.6 μg/kg, respectively. -
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