Determination of Oleandrin in Blood and Liver Samples by LC-MS/MS / 法医学杂志

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.

Determination of Triptolide and Wilforlide A in Biological Samples by LC-MS/MS / 法医学杂志

OBJECTIVE@#To determinate triptolide and wilforlide A in biological samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS) method and to verify the method.@*METHODS@#After 0.4 mL blood, urine or 0.4 g hepatic tissues with internal standard were extracted by ethyl acetate, they were separated on a Allure PFP Propyl (100 mm x 2.1 mm, 5 µm) with a mobile phase of methanol-20 mmol/L ammonium acetate using gradient elution. For mass spectrometric detection, electrospray ionization (ESI⁺) in positive mode was elected and the data was collected using multiple-reaction monitoring (MRM).@*RESULTS@#The linearity was good (r > 0.995 0) and the limit of detection was 2 ng/mL or 2 ng/g for triptolide and wilforlide A. The recovery was 61.08%-102.98%. The intra-day and inter-day precision was less than 12.58% for each biological sample, and the accuracy was 90.61%-105.80%.@*CONCLUSION@#This method is simple, convenient and good selective, and could be applied to analysis of triptolide and wilforlide A in different biological samples. And the method may provide technical support for forensic medicine identification, clinical diagnosis and treatment of tripterygium wilfordii Hook. f. poisoning.

Simultaneous screening for 45 poisonous alkaloids in blood by LC-MS/MS / 法医学杂志

OBJECTIVE@#To develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) screening method for 45 poisonous alkaloids in blood.@*METHODS@#Identification was based on the compound's retention time and two precursor-to-production transitions. The method involved a liquid-liquid extraction (LLE) followed by LC-MS/MS with multiple-reaction monitoring (MRM). When 1 mL of blood was extracted with diethyl ether at pH = 9.2 with SKF525A as the internal standard, the target compounds were analyzed with LC-MS/MS in the positive ionization mode.@*RESULTS@#The target alkaloids had good linearity (r>0.995 1), both the intra-day precision and inter-day precision being less than 14.77%. The limits of detection ranged from 0.05 to 25 ng/mL in blood.@*CONCLUSION@#The method is selective and sensitive in detecting poisonous alkaloids with a total running time of 12 minutes; therefore it was successfully applied to some actual cases of suspected alkaloids poisoning.