PDF(Pubmed)
Abstract：
Anticoagulant rodenticides (ARs) are used to control rodent populations. Poisoning of non-target species can occur by accidental consumption of commercial formulations used for rodent control. A robust method for determining ARs in animal tissues is important for animal postmortem diagnostic and forensic purposes. We evaluated an ultra-performance liquid chromatography coupled with mass spectrometry (UPLC-MS) method to quantify 8 ARs (brodifacoum, bromadiolone, chlorophacinone, coumachlor, dicoumarol, difethialone, diphacinone, warfarin) in a wide range of animal (bovine, canine, chicken, equine, porcine) liver samples, including incurred samples. We further evaluated UPLC-MS in 2 interlaboratory comparison (ILC) studies; one an ILC exercise (ICE), the other a proficiency test (PT). The limits of detection of UPLC-MS were 0.3-3.1 ng/g, and the limits of quantification were 0.8-9.4 ng/g. The recoveries obtained using UPLC-MS were 90-115%, and relative SDs were 1.2-13% for each of the 8 ARs for the 50, 500, and 2,000 ng/g spiked liver samples. The overall accuracy from the laboratories participating in the 2 ILC studies (4 and 11 laboratories for ICE and PT studies, respectively) were 86-118%, with relative repeatability SDs of 3.7-11%, relative reproducibility SDs of 7.8-31.2%, and Horwitz ratio values of 0.5-1.5. Via the ILC studies, we verified the accuracy of UPLC-MS for AR analysis in liver matrices and demonstrated that ILC can be utilized to evaluate performance characteristics of analytical methods.
摘要：
抗凝血杀鼠剂(ARs)用于控制啮齿动物种群。非目标物种的中毒可通过意外消耗用于啮齿动物控制的商业制剂而发生。用于确定动物组织中的AR的稳健方法对于动物死后诊断和法医目的很重要。我们评估了一种超高效液相色谱与质谱联用（UPLC-MS）方法来定量8种ARs（brodifacoum，溴敌隆,氯霉素,coumachlor,双香丸,difathialone,苯丙胺酮,华法林)在广泛的动物(牛，犬,鸡肉,马,猪)肝脏样本，包括发生的样品。我们在2项实验室间比较(ILC)研究中进一步评估了UPLC-MS；一项是ILC练习(ICE)，另一个是能力测试(PT)。UPLC-MS的检出限为0.3-3.1ng/g，定量限为0.8-9.4ng/g。UPLC-MS的回收率为90-115%,对于50、500和2,000ng/g加标肝脏样品，8种ARs中的每一种的相对SD为1.2-13%。参与2项ILC研究的实验室的总体准确性（ICE和PT研究的4个和11个实验室，分别)为86-118%，相对重复性SD为3.7-11%，相对重现性SDs为7.8-31.2%，和Horwitz比值为0.5-1.5。通过ILC的研究，我们验证了UPLC-MS用于肝脏基质中AR分析的准确性,并证明ILC可用于评估分析方法的性能特征.
