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液相色谱-质谱联用技术测定生物样本中的红豆杉生物碱

LC-MS determination of Taxus alkaloids in biological specimens.

作者信息

Beike J, Karger B, Meiners T, Brinkmann B, Köhler H

机构信息

Institute of Legal Medicine, University Hospital Münster, Röntgenstrasse 23, 48149, Münster, Germany.

出版信息

Int J Legal Med. 2003 Dec;117(6):335-9. doi: 10.1007/s00414-003-0399-y. Epub 2003 Oct 3.

Abstract

A semi-quantitative LC-MS method was developed for the detection of the pseudo alkaloids of Taxus baccata (yew) from human body fluids and tissue samples. This method was used to examine the cause of death of a 43-year-old man who died several hours after he drank a decoction of taxus leaves. Autopsy and histology demonstrated early signs of myocardial hypoxia. Since investigation of the stomach content did not yield evidence of taxus ingestion, the taxus alkaloids were determined in blood, stomach content and tissue samples of the deceased by LC-MS. The samples were prepared by solid phase extraction on RP-18 columns. Chromatographic separation was achieved by HPLC on a RP-8 column, coupled to an ion trap mass spectrometer (Finnigan LCQ). An atmospheric pressure electrospray ionisation was performed. Spectra of the alkaloids were recorded in the single MS mode and in the MS-MS mode and compared with reference spectra obtained from an extract of yew leaves. In the stomach content, the kidneys, the liver and a heart blood sample of the deceased, alkaloids of Taxus baccata, predominantly taxine B and iso-taxine B, were identified. The semi-quantitative evaluation of the heart blood revealed a taxine concentration of 11 micro g taxine/g. As far as we know this is the first case in which a semi-quantitative analysis of taxine alkaloids has been performed.

摘要

开发了一种半定量液相色谱-质谱法,用于检测人体体液和组织样本中的欧洲红豆杉(紫杉)假生物碱。该方法用于调查一名43岁男子的死因,该男子在饮用紫杉叶煎剂数小时后死亡。尸检和组织学显示出心肌缺氧的早期迹象。由于对胃内容物的调查未发现摄入紫杉的证据,因此通过液相色谱-质谱法测定了死者血液、胃内容物和组织样本中的紫杉生物碱。样品通过在RP-18柱上进行固相萃取制备。色谱分离通过在RP-8柱上进行高效液相色谱实现,该柱与离子阱质谱仪(Finnigan LCQ)联用。进行了大气压电喷雾电离。生物碱的光谱在单离子质谱模式和串联质谱模式下记录,并与从紫杉叶提取物获得的参考光谱进行比较。在死者的胃内容物、肾脏、肝脏和心脏血液样本中,鉴定出了欧洲红豆杉的生物碱,主要是紫杉碱B和异紫杉碱B。对心脏血液的半定量评估显示紫杉碱浓度为11微克/克紫杉碱。据我们所知,这是第一例对紫杉碱生物碱进行半定量分析的案例。

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