Institute for Chemistry and Biology of the Marine Environment, Carl von Ossietzky University of Oldenburg, Carl-von-Ossietzky-Str. 9-11, D-26129 Oldenburg, Germany.
Forensic Sci Int. 2012 Feb 10;215(1-3):146-51. doi: 10.1016/j.forsciint.2011.02.013. Epub 2011 Mar 3.
A sensitive and specific liquid chromatography tandem mass spectrometry (HPLC-ESI(+)-MS/MS) procedure was developed and validated for the identification and quantification of thevetin B and further cardiac glycosides in human serum. The seeds of Yellow Oleander (Thevetia peruviana) contain cardiac glycosides that can cause serious intoxication. A mixture of six thevetia glycosides was extracted from these seeds and characterized. Thevetin B, isolated and efficiently purified from that mixture, is the main component and can be used as evidence. Solid phase extraction (SPE) proved to be an effective sample preparation method. Digoxin-d3 was used as the internal standard. Although ion suppression occurs, the limit of detection (LOD) is 0.27 ng/ml serum for thevetin B. Recovery is higher than 94%, and accuracy and precision were proficient. Method refinement was carried out with regard to developing a general screening method for cardiac glycosides. The assay is linear over the range of 0.5-8 ng/ml serum. Finally, the method was applied to a case of thevetia seed ingestion.
建立并验证了一种灵敏且特异的液相色谱串联质谱（HPLC-ESI(+)-MS/MS）法，用于鉴定和定量人血清中的海杧果苷 B 和其他强心苷。黄夹竹桃（Thevetia peruviana）的种子含有可导致严重中毒的强心苷。从这些种子中提取并鉴定了六种海杧果苷的混合物。从该混合物中分离并有效纯化的海杧果苷 B 是主要成分，可作为证据。固相萃取（SPE）被证明是一种有效的样品制备方法。地高辛-d3 被用作内标。尽管存在离子抑制，但海杧果苷 B 的检测限（LOD）为 0.27ng/ml 血清。回收率高于 94%，准确性和精密度良好。该方法经过改进，可用于一般的强心苷筛选方法。该测定方法在 0.5-8ng/ml 血清范围内呈线性。最后，该方法应用于一例海杧果种子摄入的案例。
