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Method validation of a survey of thevetia cardiac glycosides in serum samples

机译:血清样品中藜芦the苷含量调查的方法验证

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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 0.27ng/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 0.5-8ng/ml serum. Finally, the method was applied to a case of thevetia seed ingestion.
机译:开发了灵敏且特异性的液相色谱串联质谱(HPLC-ESI + -MS / MS)程序,并经过验证,可用于鉴定和定量人血清中的维他汀B和其他强心苷。黄夹竹桃(Thevetia peruviana)的种子中含有强心苷,可能引起严重的中毒。从这些种子中提取了六种藜芦苷的混合物并进行了表征。从该混合物中分离并有效纯化的Thevetin B是主要成分,可以用作证据。固相萃取(SPE)被证明是一种有效的样品制备方法。地高辛-d3用作内标。尽管发生了离子抑制,但维维汀B的检出限(LOD)为0.27ng / ml血清。回收率高于94%,准确度和精密度均很高。关于开发强心苷的通用筛选方法进行了方法改进。该测定在0.5-8ng / ml血清范围内呈线性。最终,该方法被用于食入维氏种子的情况。

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