Shormanov V K, Kvachahija L L, Scherbakov D P, Chaplygin A V, Ljamin V N
GBOU VPO 'Kurskij gosudarstvennyj meditsinskij universitet', Kursk, Rossija, 305041.
EKTs UVD po Kurskoj oblasti, Kursk, Rossija, 305000.
Sud Med Ekspert. 2015 Mar-Apr;58(2):39-45. doi: 10.17116/sudmed201558239-45.
The objective of the present study was to determine the optimal conditions for isolation of dilthiasem, its purification by the combination of the extraction and column chromatography techniques, and the development of the universal method for the detection of this compound in the biological material. Other research methods included thin layer chromatography (TLC), gas chromatography mass-spectrometry (GH-MS), extraction, low-pressure column chromatography, and spectrophotometry. The effectiveness of dilthiasem isolation from the biological material with the use of 12 organic substances, water, and aqueous solutions was compared. The use of acetone as the universal solvent for dilthiasem isolation from the tissues and biological fluids of the cadaveric organs was substantiated. It was shown that dilthiasem can be purified from endogenous substances contained in the biological materials by means of combined liquid-liquid extraction and chromatography on the 30 mcm Silasorb C-18 column. The new modifications of thin layer chromatography and gas chromatography mass-spectrometry (GH-MS) are proposed for the identification and quantitative determination of dilthiasem isolated from cadaveric blood and hepatic tissue.
本研究的目的是确定分离双硫嗪的最佳条件,通过萃取和柱色谱技术相结合对其进行纯化,并开发在生物材料中检测该化合物的通用方法。其他研究方法包括薄层色谱法(TLC)、气相色谱 - 质谱法(GH - MS)、萃取、低压柱色谱法和分光光度法。比较了使用12种有机物质、水和水溶液从生物材料中分离双硫嗪的效果。证实了使用丙酮作为从尸体器官的组织和生物流体中分离双硫嗪的通用溶剂。结果表明,双硫嗪可通过液 - 液萃取和在30微米Silasorb C - 18柱上进行色谱分离,从生物材料中所含的内源性物质中纯化出来。提出了薄层色谱法和气相色谱 - 质谱法(GH - MS)的新改进方法,用于鉴定和定量测定从尸体血液和肝组织中分离出的双硫嗪。