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采用连续固相萃取法,随后进行液相色谱 - 电喷雾电离正离子模式串联质谱分析,对蜣螂死后及活体组织中的伊维菌素进行分离和测定。

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.

作者信息

Ortiz Antonio J, Cortez Vieyle, Azzouz Abdelmonaim, Verdú José R

机构信息

Departamento de Química Inorgánica y Química Orgánica. Universidad de Jaén, EPS de Linares. Linares, Spain.

I.U.I. CIBIO, Universidad de Alicante, Alicante, Spain.

出版信息

PLoS One. 2017 Feb 16;12(2):e0172202. doi: 10.1371/journal.pone.0172202. eCollection 2017.

Abstract

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.

摘要

一种基于溶剂萃取,随后使用聚合物吸附剂进行连续固相萃取(SPE)净化的新分析方法,被证明适用于使用液相色谱结合正电喷雾电离串联质谱(LC/ESI+-MS/MS)检测蜣螂复杂生物基质(血淋巴、排泄物或干燥组织)中的伊维菌素。以3:1的信噪比计算,在痕量水平下昆虫基质中的检测限(LOD)为0.01 ng g-1,定量限(LOQ)为0.1 ng g-1。所提出的方法成功用于在体内和死后样本中对小样本进行分析时定量测定伊维菌素水平,证明该方法对于专注于昆虫未来药代动力学和生物利用度研究以及建立新方案以研究伊维菌素对非靶节肢动物(如蜣螂和与“粪便群落”相关的其他昆虫)影响的定量分析很有用。由于在两种体内基质中均获得了令人满意的精密度和准确度值,我们建议该方法可始终用于专注于昆虫未来药代动力学和生物利用度研究的定量测定。此外,这种新分析方法成功应用于来自田间的死蜣螂的生物样本,表明该方法可用于建立昆虫尸体中伊维菌素残留的新常规分析,以补充典型的死亡率测试。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/c018/5313191/2a348734aa55/pone.0172202.g001.jpg

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