Оптимизация процедуры исследования содержания азалептина в биологических объектах методом газовой хроматографии с масс-спектрометрическим детектированием

Abstract

Purpose. Creation, based on the improvement (as applied to the use in forensic practice), of a procedure for preparing samples of biological material that is analytically more reliable than the existing ones, a method for the detection and quantitative determination of azaleptin using gas chromatography technology with mass selective detection. Material, reagent and instrumentation of the research technology. Internal organs, hair; azaleptin (tablets of the Borisov Plant of Medical Preparations containing 0.25 mg of azaleptin); methanol, isopropanol, chloroform, ethyl acetate (ethyl acetate), ammonium hydroxide (250 g / l, chemically pure grade; VetexQ reagent kits (Interlab, Russia) for the extraction of toxic substances from the internal organs of a corpse using the QuEChERS method (USA Gas chromatograph Agilent 6890N Network GC System with mass selective detector Agilent 5975C VL VSD (Agilent, USA) Scanning electron microscope (SEM) LEO-1420 (Netherlands) Laser dispersion analyzer MasterSizer 3000 (Malvern Panalylical, UK). Results. Methods have been developed for the preparation of samples of tissues of internal organs and other biological objects-hair (nails) using OU-A and AS coals as sorbents. It has been established that coal of the AC grade, containing a large number of mesopores capable of absorbing molecules, is most suitable for obtaining pure extracts from biological material. It has been shown that the use of OU-A grade activated carbon and an experimental sample of AC grade coal for purification of samples from compounds that give false positive results in the determination of azaleptin is possible when they are modified with Na-SAC. Extraction of azaleptin from blood and urine is possible due to the modification of the sorption-desorption properties of activated carbons under the action of 8% (80 g / l) Na-SAC. Conclusions: 1. Methods have been developed for the preparation of samples of tissues of internal organs and other biological objects (hair, nails) based on the use of the sorption properties of modified coals. 2. To obtain purer extracts from the biological material under study, the most suitable was the AC grade coal containing a large number of mesopores capable of absorbing molecules. 3. It has been established that the use of OU-A activated carbon and an experimental sample of AC coal as a sorbent for cleaning samples obtained from biological samples is possible in cases of their modification using Na-SAC. 4. When extracting azaleptin from biological samples, the optimal sorption-desorption properties of activated carbons are manifested with the introduction of 8% Na-SAC. 5. The use of the procedure for preparing samples of biological material for research, improved during the execution of the work, made it possible to increase the accuracy and reliability of the gas chromatographic determination of azaleptin in samples of biological objects.