Tusiewicz Kaja, Wachełko Olga, Zawadzki Marcin, Szpot Paweł
Department of Forensic Medicine, Wroclaw Medical University, Wroclaw, Poland.
Institute of Toxicology Research, Borowa, Poland.
Toxicol Mech Methods. 2024 Mar;34(3):271-282. doi: 10.1080/15376516.2023.2280212. Epub 2023 Nov 28.
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-CN 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.
一名30岁男子被发现死在房子前，已无生命迹象。该男子死后五年测定了其血液和尿液中的氰化物浓度。此外，还对一份真实案件的血液样本进行了为期730天的稳定性研究。样品制备程序包括用甲醇与水的混合物沉淀、固相萃取（SPE）以及使用五氟苄基溴（PFB-Br）进行衍生化。使用气相色谱-串联四极杆质谱（GC-QqQ-MS/MS）同位素稀释法对样品进行分析。分离使用SH-RXI-5MS柱（30 m×0.25 mm，0.25 µm）。使用带有电子电离（EI）离子源的三重四极杆质谱仪在多反应监测（MRM）模式下检测五氟苄基氰（PFB-CN）。该男子死后5年，血液中氰化物浓度为1900 ng/mL，尿液中为500 ng/mL。在该男子死后6年和7年对真实血液样本进行的稳定性研究显示，氰化物浓度分别为1898.2 ng/mL和1618.7 ng/mL。虽然分光光度法和比色法记录了氰化物浓度随时间的增减情况，但较新的色谱法主要显示浓度下降。本文所呈现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，仍需要更多的研究。
