一名30岁的男子被发现在房子前面没有生命迹象。血中和尿中的氰化物浓度是在该人死后五年测定的。更重要的是,在真实的病例血样中进行了730天的稳定性研究。样品制备程序包括用甲醇:水混合物沉淀,固相萃取(SPE)和使用PFB-Br(五氟苄基溴)进行衍生化。使用GC-QqQ-MS/MS(气相色谱-串联质谱联用)同位素稀释法分析样品。使用SH-RXI-5MS柱(30mx0.25mm,0.25µm)。PFB-CN和PFB-13CN的检测是使用具有电子电离(EI)离子源的三重四极质谱仪在多反应监测(MRM)模式下实现的。这个人死后5年,氰化物浓度为:血液中1900ng/mL,尿液中500ng/mL。在该人死亡后6年和7年的真实血液样本中进行的稳定性研究显示,氰化物浓度为1898.2ng/mL和1618.7ng/mL,分别。虽然分光光度法和比色法记录了氰化物浓度随时间的减少和增加,较新的色谱方法主要表明减少。本文提出的研究似乎证实了这一趋势。然而,为了可靠地解释生物材料中氰化物浓度的结果,更多的研究仍然是必要的。
A 30 year old man was found with no signs of life in front of the house. The cyanide concentration in blood and urine was determined five years after the man\'s death. What is more, a stability study was conducted for 730 days in an authentic casework blood sample. Sample preparation procedure included precipitation with methanol:water mixture, solid phase extraction (SPE) and derivatization with the use of PFB-Br (pentafluorobenzyl bromide). The sample was analyzed using GC-QqQ-MS/MS (gas chromatopraphy coupled with tandem mass spectrometry) isotope dilution method. Separation was done using a SH-RXI-5MS column (30 m x 0.25 mm, 0.25 µm). Detection of PFB-CN and PFB-13CN was achieved using a triple-quadrupole mass spectrometer with an electron ionization (EI) ion source in multiple reaction monitoring (MRM) mode. After 5 years from the man\'s death, cyanide concentration was: 1900 ng/mL in blood and 500 ng/mL in urine. Stability study performed in an authentic blood sample 6 and 7 years after the man\'s death revealed cyanide concentrations of 1898.2 ng/mL and 1618.7 ng/mL, respectively. While spectrophotometric and colorimetric methods recorded both decrease and increase in cyanide concentration over time, newer chromatographic methods mainly indicate a decrease. The studies presented in this paper seem to confirm this trend. However, in order to interpretate the results of cyanide concentration in biological material reliably, more research is still necessary.