ABSTRACT
Objective 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.Methods Blood or liver tissues underwent a liquidliquid extraction (LLE) using ethyl acetate, and the extract was separated on an Agilent ZORBAX SB-C18column and eluted with a gradient of acetonitrile and 20 mmol/L ammonium acetate (containing0.1％formic acid).Oleandrin was detected using electrospray positive ionization (ESI+) with multiplereaction monitoring (MRM) mode.Results Oleandrin showed excellent linearity in both blood and liver samples in the corresponding linear range (r＞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 than10.71％, 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 from65.5 to 29 600.0 ng/mL (ng/g).Conclusion 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.
ABSTRACT
Objective To establish the analytical method of oleandrin and adynerin in human blood by HPLC-MS/MS. Methods After protein sediment by acetonitril, the concentrations of oleandrin and adynerin in human blood were quantitatively determined by HPLC-MS/MS. The qualitative analysis was conducted based on retention time and MRM ions. Besides, the standard curve method was used for quantification. Results The detection limits of both oleandrin and adynerin were 0.5ng/mL, the linear range was from 1ng/mL to 1mg/mL, with a recovery rate of 75.2%~95.7%. Conclusion The detecting protocol has the advantages of high sensitivity, fast and high accuracy with a relatively wide linear range, which is especially suitable for rapid detection of oleander toxins, alexandrine and adynerin in particular, in human blood in poisoning cases.