USDA/APHIS/WS National Wildlife Research Center, Fort Collins, CO, United States of America.
USDA/APHIS/WS National Wildlife Research Center, Barrigada, GU, United States of America.
PLoS One. 2023 Aug 8;18(8):e0289261. doi: 10.1371/journal.pone.0289261. eCollection 2023.
A specific and sensitive liquid chromatography-tandem mass spectrometry method was developed and validated for the determination of the anticoagulant rodenticide diphacinone (DPN) in mouse and rat liver. Tissue samples were extracted with a mixture of water and acetonitrile containing ammonium hydroxide. The extracted sample was cleaned up with a combination of liquid-liquid partitioning and dispersive solid phase extraction. Chromatographic separation was achieved using a Waters X-Bridge BEH C-18 LC column (50 mm, 2.1 mm ID, 2.5 μm particle size) with detection on a triple quadrupole mass spectrometer in multiple reaction monitoring (MRM) mode. The monitored transition for DPN was m/z 339.0 → 167.0 for quantitation and 339.0 → 172.0 and 339.0 → 116.0 for confirmation. The linear range was 0.5 to 375 ng/mL. The average precision of DPN, represented by the relative standard deviation of the observed concentrations, was 7.2% (range = 0.97% - 20.4%) and the average accuracy, represented by the relative error, was 5.8% (range = 1.06% - 14.7%). The recovery of DPN fortified at 3 different levels averaged 106% in rat liver and 101% in mouse liver. The established method was successfully used to determine DPN residue levels in Polynesian rats (Rattus exulans) and mice (Mus musculus) fed two different formulated baits containing DPN. The observed residue levels were consistent with values observed in other rodent studies. However, the amount of bait consumed was lower for the novel baits evaluated in this study.
建立并验证了一种用于检测鼠肝和鼠肝中抗凝杀鼠剂敌鼠（DPN）的特异性和灵敏的液相色谱-串联质谱法。组织样品用含氨的水和乙腈的混合物提取。提取的样品经液-液分配和分散固相萃取净化。采用 Waters X-Bridge BEH C-18 LC 柱（50mm，2.1mmID，2.5μm粒径）进行色谱分离，在三重四极杆质谱仪上以多反应监测（MRM）模式进行检测。用于定量的 DPN 的监测转换为 m/z 339.0→167.0，用于确证的监测转换为 m/z 339.0→172.0 和 339.0→116.0。线性范围为 0.5 至 375ng/mL。DPN 的平均精密度（以观察浓度的相对标准偏差表示）为 7.2%（范围为 0.97%至 20.4%），平均准确度（以相对误差表示）为 5.8%（范围为 1.06%至 14.7%）。在大鼠肝和小鼠肝中，3 个不同水平添加的 DPN 的平均回收率分别为 106%和 101%。该方法成功用于测定食用两种不同含敌鼠配方诱饵的波利尼西亚大鼠（Rattus exulans）和小鼠（Mus musculus）中的 DPN 残留水平。观察到的残留水平与其他啮齿动物研究中观察到的值一致。然而，在本研究中评估的新型诱饵的消耗的诱饵量较低。
