Guo Hao, Wang Junwei, Wu Yuhong, Liu Wenwen, Bu Juan, Zhao Qingbiao
Chongqing Institute of Forensic Science, Chongqing, China.
Department of Forensic Science and Technology, Chongqing Police College, Chongqing, China.
J Anal Toxicol. 2018 Sep 1;42(7):459-466. doi: 10.1093/jat/bky024.
A sensitive and rapid method for the simultaneous determination of nine anticoagulant rodenticides (ARs) in human blood is reported herein. The method involves phospholipid removal pretreatment for reduced matrix effect (ME) and detection with ultra-performance liquid chromatography coupled with tandem mass spectrometry. Satisfactory recoveries were achieved ranging from 80.6% to 113.1% for the nine analytes, with the intra-day relative standard deviations (RSDs) in the range of 3.4-7.9% and inter-day RSDs in the range of 4.1-8.3%, indicating good precision. Linear relationships with correlation coefficients above 0.998 (n = 6) were found in the range of 1-2,000 ng/mL. High sensitivity was achieved with limits of detection ranging from 0.02 to 0.3. The application of phospholipid removal step significantly optimized the ME, and the reduction of ME ranged from 6.1% to 15.5%. This method was successfully applied to the determination of ARs for blood samples from real forensic cases. These results prove that this method is reliable for rapid forensic and clinical diagnosis. The removal capabilities for five representative phospholipids that are abundant in blood were evaluated individually with Phree™ phospholipid removal plates. While significant capabilities for phospholipid removal were confirmed, the results showed that the removal capability for certain phospholipid could be improved.
本文报道了一种灵敏、快速同时测定人血液中九种抗凝血灭鼠剂(ARs)的方法。该方法包括用于降低基质效应(ME)的磷脂去除预处理,以及采用超高效液相色谱-串联质谱法进行检测。九种分析物的回收率令人满意,在80.6%至113.1%之间,日内相对标准偏差(RSDs)在3.4 - 7.9%范围内,日间RSDs在4.1 - 8.3%范围内,表明精密度良好。在1 - 2000 ng/mL范围内发现了相关系数高于0.998(n = 6)的线性关系。检测限在0.02至0.3之间,实现了高灵敏度。磷脂去除步骤的应用显著优化了基质效应,基质效应的降低范围为6.1%至15.5%。该方法成功应用于实际法医案件血液样本中ARs的测定。这些结果证明该方法对于快速法医和临床诊断是可靠的。使用Phree™磷脂去除板分别评估了血液中丰富的五种代表性磷脂的去除能力。虽然确认了显著的磷脂去除能力,但结果表明某些磷脂的去除能力可以提高。