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Isolation and determination of ivermectin in post-mortem and in vivo tissues of dung beetles using a continuous solid phase extraction method followed by LC-ESI+-MS/MS

机译:连续固相萃取-LC-ESI + -MS / MS法分离并测定粪甲虫尸体和体内组织中的伊维菌素

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摘要

A new analytical method based on solvent extraction, followed by continuous solid-phase extraction (SPE) clean-up using a polymeric sorbent, was demonstrated to be applicable for the detection of ivermectin in complex biological matrices of dung beetles (hemolymph, excreta or dry tissues) using liquid chromatography combined with positive electrospray ionization tandem mass spectrometry (LC/ESI+–MS/MS). Using a signal-to-noise ratio of 3:1, the limit of detection (LOD) in the insect matrices at trace levels was 0.01 ng g–1 and the limit of quantification (LOQ) was 0.1 ng g–1. The proposed method was successfully used to quantitatively determine the levels of ivermectin in the analysis of small samples in in vivo and post mortem samples, demonstrating the usefulness for quantitative analyses that are focused on future pharmacokinetic and bioavailability studies in insects and the establishment of a new protocol to study the impact of ivermectin on non-target arthropods such as dung beetles and other insects that are related with the “dung community”. Because satisfactory precision and accuracy values were obtained in both in vivo matrices, we suggest that the method can be consistently used for quantitative determinations that are focused on future pharmacokinetic and bioavailability studies in insects. Furthermore, this new analytical method was successfully applied to biological samples of dead dung beetles from the field suggesting that the method can be used to establish a new routine analysis of ivermectin residues in insect carcasses that is applied to complement typical mortality tests.
机译:一种新的基于溶剂萃取的分析方法,然后使用聚合物吸附剂进行连续固相萃取(SPE)净化,被证明可用于检测粪甲虫的复杂生物基质(血淋巴,排泄物或干物质)中的伊维菌素。液相色谱结合正电喷雾电离串联质谱(LC / ESI + –MS / MS)。使用3:1的信噪比,在痕量水平下昆虫基质中的检出限(LOD)为0.01 ng g –1 ,定量限(LOQ)为0.1 ng g –1 。所提出的方法已成功用于定量测定体内和尸体样本中小样本样品中伊维菌素的水平,证明了定量分析的有用性,该定量分析侧重于昆虫的未来药代动力学和生物利用度研究,并建立了新的方法。协议,研究伊维菌素对非目标节肢动物(例如,甲虫和其他与“粪便群落”有关的昆虫)的影响。因为在两种体内基质中均获得了令人满意的精度和准确度值,所以我们建议该方法可始终用于定量测定,重点是对昆虫的未来药代动力学和生物利用度研究。此外,这种新的分析方法已成功应用于野外死粪甲虫的生物样品,表明该方法可用于建立昆虫尸体中伊维菌素残留物的新常规分析方法,以补充典型的死亡率测试。

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