Zhai J X, Yan H, Shen M, Shen B H, Liu W
Shanghai Key Laboratory of Forensic Medicine, Shanghai Forensic Service Platform, Academy of Forensic Science, Shanghai 200063, China.
Institute of Forensic Medicine and Laboratory Medicine, Jining Medical University, Jining 272067, Shandong Province, China.
Fa Yi Xue Za Zhi. 2018 Jun;34(6):585-589. doi: 10.12116/j.issn.1004-5619.2018.06.002. Epub 2018 Dec 25.
To develop a liquid chromatography-tandem mass spectrometry （LC-MS/MS） analytical method for the determination of oleandrin in blood and liver tissues, which could be applied to the cases of death caused by oleander poisoning.
Blood or liver tissues underwent a liquid-liquid extraction （LLE） using ethyl acetate, and the extract was separated on an Agilent ZORBAX SB-C column and eluted with a gradient of acetonitrile and 20 mmol/L ammonium acetate （containing 0.1% formic acid）. Oleandrin was detected using electrospray positive ionization （ESI+） with multiple-reaction monitoring （MRM） mode.
Oleandrin showed excellent linearity in both blood and liver samples in the corresponding linear range （>0.995 0）, with detection limits 1 ng/mL and 2 ng/g, respectively, extraction recovery rates greater than 70.50%, both intra- and inter-day precisions less than 10.71%, accuracies 98.42%-111.63%, and matrix effects 91.52%-106.39%. The method was successfully applied to a case of suspected oleander poisoning. Oleandrin was detected in the blood, urine, liver tissues, bile, stomach wall tissues and stomach contents of the cadaver, with the content ranging from 65.5 to 29 600.0 ng/mL （ng/g）.
The method developed in this study is simple and convenient to operate with good selectivity, and is suitable for the analysis of oleandrin in biological samples such as blood and liver tissues, which can provide technical support for forensic identification and clinical diagnosis and treatment of oleander poisoning.
建立一种液相色谱-串联质谱（LC-MS/MS）分析方法，用于测定血液和肝组织中的夹竹桃苷，该方法可应用于夹竹桃中毒致死案件。
血液或肝组织采用乙酸乙酯进行液液萃取（LLE），萃取液在安捷伦ZORBAX SB-C柱上分离，并用乙腈和20 mmol/L乙酸铵（含0.1%甲酸）梯度洗脱。夹竹桃苷采用电喷雾正离子化（ESI+）和多反应监测（MRM）模式进行检测。
夹竹桃苷在相应线性范围内在血液和肝样本中均显示出良好的线性（>0.995 0），检测限分别为1 ng/mL和2 ng/g，萃取回收率大于70.50%，日内和日间精密度均小于10.71%，准确度为98.42%-111.63%，基质效应为91.52%-106.39%。该方法成功应用于1例疑似夹竹桃中毒案件。在尸体的血液、尿液、肝组织、胆汁、胃壁组织和胃内容物中检测到夹竹桃苷，含量范围为65.5至29 600.0 ng/mL（ng/g）。
本研究建立的方法操作简单方便，选择性好，适用于血液和肝组织等生物样本中夹竹桃苷的分析，可为夹竹桃中毒的法医学鉴定及临床诊断治疗提供技术支持。
