猛禽類肝臟中抗凝血殺鼠劑多重殘留分析方法之建立及應用

Analytical Method for the Determination of Residual Anticoagulant Rodenticides in Raptorial Bird Livers

陳慧珊(Hui-Shan Chen) ； 徐慈鴻(Tsyr-Horng Shyu)

《臺灣農藥科學》 6期 (2019/06) Pp. 105-117

https://doi.org/10.6671/TPS.201906_(6).05

摘要

本研究建立猛禽類肝臟中抗凝血殺鼠劑多重殘留檢驗分析技術。肝臟樣品經均質後以乙腈萃取，加入氯化鈉經離心分層後，取上層液再以乙腈飽和之正己烷進行淨化程序，最後以液相層析串聯式質譜儀進行定性及定量分析；於肝臟樣品分別添加0.02μg／g及0.1μg／g的殺鼠劑進行回收率試驗， 結果顯示包括可滅鼠（brodifacoum）、撲滅鼠（bromadiolone）、可伐鼠（chlorophacinone）、coumachlor、coumafuryl、剋滅鼠（coumatetralyl）、雙滅鼠（difenacoum）、達滅鼠（difenthialone）、得伐鼠（diphacinone）、伏滅鼠（dlocoumafen）、pindone、valone及殺鼠靈（warfarin）等13種抗凝血殺鼠劑之低濃度（0.02μg／g）的平均回收率為70～97%，重複性試驗之變異係數在1～20%間，而高濃度（0.1μg／g）的平均回收率為66～102％，重複性試驗之變異係數在2～16%間，方法定量極限為0.002～0.005μg／g，顯示本分析方法之建立，可快速準確的進行猛禽類肝臟中抗凝血殺鼠劑殘留檢測之定性及定量，應用本方法檢測死亡猛禽肝臟中抗凝血殺鼠劑，檢出藥劑為可滅鼠、伏滅鼠、撲滅鼠及雙滅鼠，可提供農藥及環境用藥主管機關參考。

關鍵字

猛禽類 ； 肝臟 ； 抗凝血殺鼠劑 ； 液相層析串聯式質譜儀

並列摘要

In order to investigate the secondary poisoning of anticoagulant rodenticidesto raptorial birds in farmland and surrounding areas, an analytical methods was developed to detect rodenticide residues in bird livers. The liver samples were homogenized and extracted with acetonitrile. After adding sodium chloride, centrifuged, the supernatant was clean up by acetonitrile-saturated hexane. Finally, qualitative and quantitative analysis was performed by liquid chromatography tandem mass spectrometer (LC-MS/MS). The average recovery of low concentrations (0.02 μg/g) of 13 rodenticides (brodifacoum, bromadiolone, chlorophacinone, coumachlor, coumafuryl, coumatetralyl, difenacoum, difenthialone, diphacinone, flocoumafen, pindone, valone and warfarin) was 70%-97%, the coefficient of variation (CV) of the repeatability test ranged from 1% to 20%, while the average recovery of the high concentration (0.1 μg/g) ranged from 66% to 102%, and the coefficient of variation (CV) of the repeatability test ranged from 2% to 16%. The limits of quantitation were 0.002~0.005 μg/g. Moreover, our method was simple and accurate for both quantitative and qualitative determination of anticoagulant rodenticides.Four rodenticides were detected in the liver of poisoned raptors. These were brodifacoum, bromadiolone, difenacoum and flocoumafen. This method can be used as a toolfor the investigation of secondary poisoning of anticoagulant rodenticides and to strengthening furtherly the management of the regulatory authorities.

並列關鍵字

raptorial birds ； liver ； anticoagulant rodenticides ； LC-MS/MS