首页> 外文期刊>Journal of Analytical Toxicology >Validation of a new liquid chromatography- tandem mass spectrometry ion-trap technique for the simultaneous determination of thirteen anticoagulant rodenticides, drugs, or natural products.
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Validation of a new liquid chromatography- tandem mass spectrometry ion-trap technique for the simultaneous determination of thirteen anticoagulant rodenticides, drugs, or natural products.

机译:验证了同时测定十三种抗凝血灭鼠剂,药物或天然产物的新型液相色谱-串联质谱离子阱技术。

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摘要

The purpose of this study was to develop and validate a liquid chromatography-tandem mass spectrometry method for the identification and quantification of anticoagulant (anti-vitamin K or AVK) compounds, including rodenticides, drugs, and natural products because no published method could be found. The proposed method is based on ion-trap technology with electrospray ionization (ESI) and multiple reaction monitoring (MRM) technique. Each AVK is identified by means of its retention time, precursor ion, and two product ions. Plasma samples are extracted by liquid-liquid partition on Toxi-tube B((R)). The method was validated on dog plasma and gave good results in terms of specificity, linearity, and percent recovery for the 14 AVK tested (warfarin, acenocoumarol, bromadiolone, brodifacoum, chlorophacinone, coumatetralyl, dicoumarol, difenacoum, difethialone, flocoumafen, fluindione, phenindione, and tioclomarol). The limits of detection ranged from 5 to 25 ng/mL. Intraday repeatability was good, but interday repeatability was more variable though still sufficient for our diagnostic purposes. The technique was successfully applied in a series of clinical investigations to demonstrate its applicability in various animal species and gave very high sensitivity and specificity results.
机译:这项研究的目的是开发和验证一种液相色谱-串联质谱法,用于鉴定和定量抗凝血(抗维生素K或AVK)化合物,包括灭鼠剂,药物和天然产物,因为找不到公开的方法。所提出的方法基于具有电喷雾电离(ESI)和多反应监测(MRM)技术的离子阱技术。每个AVK均通过其保留时间,前体离子和两个产物离子来识别。通过在Toxi-tube B(R)上进行液-液分配来提取血浆样品。该方法已在狗血浆上进行验证,并且针对14种经测试的AVK(华法林,乙酰香豆酚,溴地丁酮,溴地芬,氯苯丙酮,香豆醛,双香豆酚,地非那草,地非噻酮,氟可那芬,氟吲哚,苯并菲宁)在特异性,线性和回收率方面均取得了良好的结果。和噻氯普洛尔)。检出限为5至25 ng / mL。日内重复性良好,但日间重复性变化更大,尽管仍足以满足我们的诊断目的。该技术已成功应用于一系列临床研究中,证明了其在各种动物物种中的适用性,并给出了很高的灵敏度和特异性结果。

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