DEVELOPMENT AND VALIDATION OF PROCEDURES FOR FORENSIC CHEMICAL DETERMINATION OF BENSULTAP

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DOI: https://doi.org/10.29296/25419218-2018-05-02
Issue: 
5
Year: 
2018

Yu.N. Baranov, V.K. Shormanov, E.A. Kovalenko, M.V. Rymarova Kursk State Medical University, 3, K. Marx St., Kursk 305004, Russian Federation

Introduction. The insecticide 2-dimethylamino-1,3-bis-(phenylsulfonyl)-propane or bensultap, a substance included in the group of biologically active compounds with anticholinesterase activity, has been effectively used in plant cultivation for a long time. This substance exhibits toxic properties against warm-blooded organisms. There are numerous cases of human poisoning, including those with a lethal outcome. The important forensic chemical value of this compound necessitates a study of the issues of its isolation from biomaterials, purification, and determination in the extracts from biomatrices. Objective: to develop and validate a procedure for the forensic chemical determination of 2-DMA-1,3-bis-(PSP)P. Material and methods. The investigation object was DMA-1,3-bis-(PSP)P; the content of the main component is ≥97%. The substance was isolated from its model mixtures with liver tissue via infusion with ethyl acetate. TLC analysis was carried out on Sorbfil plates; the mobile phase was hexane-dioxane-propanol-2-acetone; an UV detector was applied. A macrocolumn adsorption chromatography was used to develop a purification scheme. Optical density was measured on a SP-46 spectrophotometer. The concentration of 2-DMA-1,3-bis-(PSP)P was determined using the equation of the calibration curve. High-performance liquid chromatography (HPLC) was employed to identify and quantify the compound in question. Results. The investigators studied the impact of the duration of contact of an insulating liquid with a biomaterial, the multiplicity of infusion, the quantitative ratio of the insulating agent and the biological object on the degree of extraction of this compound from the biological material with an optimal insulating agent. The relationship of the degree of extraction of 2-DMA-1,3-bis-(PSP)P to its level in the biological matrix was studied under the optimal conditions found. Conclusion. A scheme for examining organ tissues and blood has been proposed to confirm that they contain 2-DMA-1,3-bis-(PSP)P via isolation with ethyl acetate, purification in the column packed with silica gel L 40/100 µm, identification and quantification using HPLC. The detection and quantification limits are 2.5 and 3.125 µg/g of biomaterial, respectively. The procedure is validated.
Keywords: 
2-dimethylamino-1
3-bis-(phenylsulfonyl)-propane (bensultap)
isolation
purification
identification
determination
validation
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