临床干血斑样本中12种抗凝血鼠药的液相色谱-串联质谱法同时定量检测

发布时间：2018-02-22 21:59

  本文关键词： 干血斑 抗凝血杀鼠药 液相色谱-串联质谱法 临床中毒快检　出处：《分析测试学报》2017年11期 　论文类型：期刊论文

【摘要】：为应对临床中毒快检的需求,建立了干血斑样本中12种抗凝血鼠药的液相色谱-串联质谱定性定量方法。针对全打孔的干血斑样本,考察了滤纸卡种类、润湿步骤、提取溶剂种类对提取效果的影响。采用C18色谱柱进行分离,以乙酸铵(5 mmol/L)水溶液-乙酸铵(5 mmol/L)甲醇溶液为流动相进行梯度洗脱,在电喷雾负离子电离方式下使用三重四极多反应监测模式检测。结果表明,采用Whatman903滤纸卡为基底,以水为溶剂充分润湿,再以含内标的甲醇溶液提取5 min,各鼠药的提取率为66%~115%,且结果稳定(日内RSD小于15%)。除杀鼠酮的线性范围为20~500 ng/m L(r2=0.998 7)外,其它11种鼠药的线性范围为5~500 ng/m L(r2=0.998 8~0.999 6);12种鼠药的回收率为61%~105%,基质效应为71%~193%(日内RSD小于15%)。该方法准确、灵敏、快速且操作简便,成功应用于3例临床鼠药中毒病人样本的快速检测,为临床毒物检测和法医毒物分析的快速筛查和准确定量提供了新的技术方法。
[Abstract]:In order to meet the requirement of rapid detection of clinical poisoning, a qualitative and quantitative method of liquid chromatography-tandem mass spectrometry (LC-MS) for 12 kinds of anticoagulant rodents in dry blood spot samples was established. C18 chromatographic column was used for separation. The mobile phase was gradient elution with ammonium acetate 5 mmol / L aqueous solution and ammonium acetate 5 mmol / L methanol solution as mobile phase. The triple quadrupole multipole reaction monitoring mode was used in the electrospray anion ionization mode. The results showed that the Whatman903 filter card was used as the substrate and the water as the solvent to fully wetting. The extraction rate of each rodenticide was 660.115 and the results were stable (RSD < 150.The linear range of rodentione was 200.500 ng/m / L ~ (2 +) 0.998 / 7). The linear range of the other 11 kinds of rodenticide was 5 #number0# ng/m / L ~ (0.998) 8 ~ 0.999 ~ (6) C ~ (12). The recovery rate of 12 kinds of rodenticide was 61 ~ 10 ~ 5 and the matrix effect was 71 ~ 1 ~ 19 ~ 3 ~ (th) (RSD was less than 1595). The method was accurate, sensitive, rapid and easy to operate. It has been successfully applied to the rapid detection of 3 clinical rodent poisoning patients, which provides a new technical method for rapid screening and accurate quantitative analysis of clinical poison and forensic toxicology.
【作者单位】： 军事医学科学院毒物药物研究所抗毒药物与毒理学国家重点实验室;军事医学科学院附属医院中毒救治科;
【基金】：全军医学科技“十三五”重大项目(AWS15J007))
【分类号】：O657.63;R99
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