应用 LC-ESI/MS/MS 测定人血中的溴敌隆和溴鼠灵及其在四起超级抗凝血类杀鼠剂中毒案件中的应用。
Determination of bromadiolone and brodifacoum in human blood using LC-ESI/MS/MS and its application in four superwarfarin poisoning cases.
机构信息
Department of Forensic Science, Shanghai Medical College, Fudan University, Shanghai 200032, China.
出版信息
Forensic Sci Int. 2012 Oct 10;222(1-3):313-7. doi: 10.1016/j.forsciint.2012.07.008. Epub 2012 Aug 19.
Superwarfarin poisoning is a growing health problem. A sensitive and reproducible LC-ESI/MS/MS (liquid chromatography electrospray ionization tandem mass spectrometry) method was developed and validated for the determination of bromadiolone and brodifacoum, the most commonly used superwarfarins, in human blood using warfarin-D5 as an internal standard. Bromadiolone and brodifacoum were extracted from whole blood samples by liquid-liquid extraction with ethyl acetate. Multiple-reaction monitoring (MRM) was used to detect bromadiolone and brodifacoum using precursor→product ion combinations of m/z 525→250 and 521→135, respectively. The calibration curves were linear (r(2)=0.9999) in the concentration range of 0.5-100.0 ng/mL for bromadiolone and brodifacoum, with a lower limit of detection of 0.1 and 0.2 ng/mL, respectively, in whole blood. This method detected trace levels of bromadiolone and brodifacoum in whole blood samples and can be used in the diagnosis of poisoned human beings.
超级杀鼠剂中毒是一个日益严重的健康问题。本研究开发并验证了一种灵敏且重现性良好的 LC-ESI/MS/MS（液相色谱-电喷雾电离串联质谱）方法，用于检测人血中溴敌隆和溴鼠灵（最常用的超级杀鼠剂），检测时以华法林-D5 作为内标。溴敌隆和溴鼠灵采用乙酸乙酯液液萃取法从全血样品中提取。采用多反应监测（MRM）模式，通过 m/z 525→250 和 521→135 分别检测溴敌隆和溴鼠灵的前体→产物离子对。溴敌隆和溴鼠灵的校准曲线在 0.5-100.0ng/mL 浓度范围内呈线性（r(2)=0.9999），在全血中的检测限分别为 0.1 和 0.2ng/mL。该方法能够检测全血样本中痕量的溴敌隆和溴鼠灵，可用于诊断中毒患者。
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