Section for Toxicology and Drug Analysis, Department of Forensic Medicine, Aarhus University, Aarhus N, Denmark.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Apr 1;879(11-12):727-36. doi: 10.1016/j.jchromb.2011.02.010. Epub 2011 Feb 13.
A liquid-chromatography-tandem-mass-spectrometry method using pneumatically assisted electrospray ionisation (LC-ESI-MS/MS) was developed for the simultaneous determination of cathinone, methcathinone, ethcathinone, amfepramone, mephedrone, flephedrone, methedrone, methylone, butylone, cathine, norephedrine, ephedrine, pseudoephedrine, methylephedrine and methylpseudoephedrine in human live and post-mortem whole blood. The blood proteins were precipitated by the addition of methanol, and the extract was purified by ultrafiltration. The separation of diastereomeric ephedrines was achieved on an ethyl-linked phenyl column. Matrix-matched calibrants combined with the isotope dilution of selected substances were used for quantitative analysis. The relative intra-laboratory reproducibility standard deviations were generally better than 7% at concentrations of 20 μg/L, and the mean true recoveries were 87-106% in the concentration range of 10-250 μg/L. The detection limits were in the range of 0.5-3 μg/L. The cathinones were unstable in whole blood and sample extracts under neutral conditions, but the stability could be improved by the acidification of the sample matrix.
建立了一种采用气动辅助电喷雾电离（LC-ESI-MS/MS）的液相色谱-串联质谱法，用于同时测定人血液中苯丙胺、甲卡西酮、乙基甲卡西酮、苯甲曲秦、氯胺酮、甲氧基甲基苯丙胺、甲基苯丙胺、丁基苯丙胺、卡西酮、去甲伪麻黄碱、麻黄碱、伪麻黄碱、甲基麻黄碱和甲基伪麻黄碱。向血液中加入甲醇沉淀蛋白，然后用超滤法对提取液进行净化。采用乙基键合的苯基柱实现了对立体异构体麻黄碱的分离。基质匹配校准物与选定物质的同位素稀释相结合用于定量分析。在浓度为 20 μg/L 时，相对实验室内重复性标准偏差通常优于 7%，在浓度为 10-250 μg/L 范围内，平均真实回收率为 87-106%。检测限在 0.5-3 μg/L 范围内。在中性条件下，血液和样品提取物中的苯丙胺不稳定，但可以通过酸化样品基质来提高稳定性。
