[Determination of 2,4-dimethylhydroxybenzene by chromatographic methods in forensic toxicological research of biological material]. / Opredelenie 2,4-dimetilgidroksibenzola khromatograficheskimi metodami pri khimiko-toksikologicheskom issledovanii biologicheskogo materiala.

OBJECTIVE: Is to develop a method for determining 2.4-dimethylhydroxybenzene (2.4-DMHOB) in biological material. The analytical methods used in the experiments were extraction, column chromatography of normal pressure, TLC, GC-MS and HPLC. To extract the analyte from the bioactive matrix, maceration with the binary insulating agent acetone-ethyl acetate (3:7) was used, observing the 2:1 mass ratio of the «insulating agent-matrix¼. Optimal conditions of semi-preparative analyte chromatography were achieved in column (150×10 mm) of «Silasbor¼ S-18 sorbent in elution with a mixture of acetonitrile-water (7:3), which was used in the proposed cleaning scheme, combining extraction and reversed-phase column chromatography. The application of the mobile phase of tetrachloromethane-dioxane (9.5:0.5) has been substantiated for the selective determination of 2.4-DMHOB by TLC («Sorbfil¼ plates). The expediency of confirming identification of the analyte in the form of 2.4-dimethyltrymethylsilylphenol using GC-MS (DB-5MS EVIDEX column (25.000×0.2 mm), stationary phase (5%-phenyl)-methylpolysiloxane, carrier gas - helium) has been shown. The group of characteristic particles in the mass spectrum of trimethylsilyl analyte derivative was represented by 45; 59; 73; 82; 91; 105; 119; 135; 149; 163; 179; 194 m/z ions. HPLC (Discovery C18 250×4.6 mm column, eluting liquid - acetate buffer solution with pH 5.5 - acetonitrile, 50:50) was used to confirm the identification and quantification of 2.4-DMHOB. A method for determining 2.4-DMHOB by the HPLC method in biological material (liver tissue) is proposed, which corresponds to the criteria of linearity, selectivity, accuracy, precision and stability. The minimum detectable quantity of 2.4-DMHOB in the bioactive matrix is 0.5 µg/g, the minimum determined quantity is 1.2 ug/g.

[Development of 2,4,6-trinitrophenol examination methods to evaluate the features of its distribution in warm-blooded animals]. / Razrabotka metodik issledovaniya 2,4,6-trinitrofenola dlya otsenki kharaktera ego raspredeleniya v organizme teplokrovnykh zhivotnykh.

THE OBJECTIVE: Is to study a 2, 4, 6-trinitrophenol (2.4,6-TNP) distribution in warm-blooded animals using physical chemical analysis methods after intragastric injection of toxicant. The methods of thin-layer chromatography, spectrophotometry and high-efficient liquid chromatography were used in the study process. Four-months-old rats of the Wistar line (males) were considered as a model of warm-blooded organisms. The investigated substance in amount of three-times LD50 was intragastrically injected in the aqueous-suspension state. 2.4,6-TNP was isolated by a mixture of acetone-acetonitrile (1:1) in a double (by 0.5 of hour) infusing mode from the bioactive matrix of experimental animals, sustaining the mass ratio of isolated agent to bioactive matrix equaled to 2:1. Purification and preliminary identification of analyte were conducted on «Sorbfil¼ plates (mobile phase - acetone - chloroform (7:3)), confirming identification - by absorption in dimethylformamide medium and by retention time in column (64×2 mm) of «Separon C-18¼ sorbent during elution by acetonitrile-water (2:8) mixture. The evaluation of 2, 4, 6-trinitrophenol quantitative content by optical density of dimethylformamide solution of analyte at 379 nm was carried out. The analyte in unchanged form was found in blood, parenchymatous and hollow organs, their contents and blood of experimental animals. The highest content of 2.4,6-TNP (mg/100 gr) was revealed in gastric content (149.88±22.70), gastric tissue (97.89±4.86), blood (15.91±0.90) and muscles (10.87±1.91).

[Lercanidipine distribution in warm-blooded animals]. / Raspredelenie lerkanidipina v organizme teplokrovnykh zhivotnykh.

THE AIM OF THE STUDY: Is to investigate the lercadipine distribution in warm-blooded animals (rats). The experimental study used rats of Wistar race. TLC, GC-MS and UV-spectrophotometry methods were used for physical and chemical analysis. Semilethal (890 mg/kg) dose of lercadipine, previously suspended in water, was injected into stomach of laboratory animals. Examined substance was isolated from the thick tissues and animals' blood by acetone, cleaned with a change of solvent and macrocolumn chromatography using 30 µm «Silasorb S-18¼ sorbent and acetonitrile-water (8:2) polar eluent. The analyte was identified by chromatographic behavior in the thin sorbent layer, retention time and set of positive ions in its mass spectrum, as well as by UV-spectrum. The analyte was determined quantitatively in bioactive matrix using UV-spectrophotometry. The methods were validated by criteria of linearity, selectivity, accuracy, precision, detection limits and quantitative determination. The main content of lercanidipine (mg/100 g) was determined in the stomach content (198.183±29.541), the stomach (195.312±21.579), the small intestine (47.096±3.947), the spleen (38.952±3.532) and the liver (26.211±2.232).

[Study of 2,6-di(propan-2-yl)phenol stability in biomaterial]. / Izuchenie ustoichivosti 2,6-di(propan-2-il)fenola v biologicheskom materiale.

The aim of this study is to research the stability of 2.6-di(propan-2-yl)phenol in biomaterial. GC-MS (column DB-5MS EVIDEX (25 m×0.2 mm); stationary liquid phase of 5%-phenyl-95% dimethylpolysiloxane), TLC (Sorbfil plates, mobile phase of hexane-diethyl ether (9:1) and spectrophotometry (solvent medium - 95% ethanol) were used as methods of analysis. 2.6-di(propan-2-yl)phenol was isolated from the biomatrix (liver tissue) by infusion with a mixture of ethyl acetate-acetone (7:3). The analyte was purified by combining extraction (water-ethyl acetate system) and semi-preparative chromatography on a column of silica gel L 40/100 µm, eluent - hexane-acetone (7:3). It was found that at -22 °C, 0 °C, 12 °C, 20 °C and 30 °C 2.6-di(propan-2-yl)phenol can be present in the liver tissue for 119, 98, 70, 56 and 42 days, respectively. The possibility of mathematical description of analyte decomposition dynamics in biomaterial (liver tissue) at the considered temperatures on the basis of hyperbola equation has been studied. The experimentally calculated coefficients in the hyperbola equation (km) for temperatures -22 °C, 0 °C, 12 °C, 20 °C and 30 °C are equal to 1823, 1130, 697, 510, and 255, respectively. The dependence km on the conserving temperature (tо) was educed. The equation for the description of dependence is offered: km=30.61∙(50-to)-402.39. It is shown that this equation can be the basis for prediction of 2.6-di(propan-2-yl)phenol stability in biomaterial (liver tissue) in the temperature range from -22 °C to 30 °C.

[Propofol: use, toxicology and assay features]. / Propofol: primenenie, toksikologicheskaya kharakteristika i osobennosti opredeleniya.

The study objective is to review the literature on the use, pharmacological properties, toxicology, and assay methods for intravenous anesthetic propofol. The scope and forms of propofol use, its pharmacokinetics, biotransformation features, which occurs more than 90% in the liver, and side effects associated with propofol use for anesthesia, are addressed. Propofol infusion syndrome (also known as PrIS) and deaths from propofol overdose due to medical errors, abuse, suicide attempts, and homicide are reported. Propofol identification and assay methods based on high-performance liquid chromatography (HPLC), gas chromatography with mass spectrometry (GC-MS), and liquid chromatography (LC) are described. The features of the methods performance are outlined; biological materials (the study objects) are listed: mainly blood and plasma, as well as urine, bile, hair, etc. The relevance of a comprehensive forensic chemical study of propofol is indicated, though there are few forensic studies of propofol.

[Amlodipine assay conditions and stability in biological material]. / Izuchenie uslovii opredeleniya i kharaktera ustoichivosti amlodipina v biologicheskom materiale.

The objective of the study is to determine amlodipine assay conditions and stability in biological material. Thin layer chromatography (TLC), gas chromatography-mass spectrometry (GC-MS) and UV-spectrophotometry were used for identification. Amlodipine was recovered from biomaterial by double (30 min each) infusing with acetone at the ratio of recovery solution and sample 2:1 (w/w). The purification was carried out by extraction and chromatography in a semi-preparative column with reverse-phase packing material Silasorb C-18 using acetone/water eluent (8:2). Amlodipine assay was performed by TLC [Sorbfil plates, butanol/acetone (5:5) as a mobile phase], GC-MS (HP-5 ms Ultra inert column (30 m×0.25×0.25 µm) with stationary phase of 5% phenyl-95% dimethyl polysiloxane), UV-spectrophotometry (95% ethanol as a solvent). The proposed assay method for amlodipine in biomaterial (liver tissue) is validated for linearity, selectivity, accuracy and precision. The amlodipine stability in model mixtures with liver tissue was studied. It was shown that the analyte stability in biological material decreases with increasing temperature. Amlodipine is stable at -25 °C, 0-2 °C, 8-10 °C, 18-22 °C, and 36 °C for 120, 112, 105, 91, and 77 days, respectively.

[Study of the stability of 2-methoxy-4-(2-propenyl) hydroxybenzene in biological material]. / Izuchenie ustoichivosti 2-metoksi-4-(2-propenil) gidroksibenzola v biologicheskom materiale.

The purpose of this work is to study the stability of 2-methoxy-4-(2-propenyl)hydroxybenzene [2-MO-4-(2-P)HOB] in biological material. For analysis, gas chromatography-mass spectrometry (GC-MS) was used: column DB-5MS EVIDEX (25 m × 0.2 mm) with a stationary phase of 5%-phenyl-95%-dimethylpolysiloxane; thin layer chromatography (TLC): Sorbfil plates, hexane-dioxane-propanol-2 mobile phase (40:5:1) and UV spectrophotometry (solvent - 95% ethanol). 2-MO-4-(2-P)HOB was isolated from the biomatrix (liver tissue) by infusion with a mixture of ethyl acetate-acetone (7:3). Purification of the analyte was carried out by combining extraction (water-ethyl acetate system) and semi-preparative column chromatography [sorbent - silica gel L 40/100 µm, eluent - hexane-dioxane (8.5:1.5)]. It was established that at -22 °C, 4 °C, 12 °C, 20 °C and 30 °C 2-MO-4-(2-P)HOB is stored in the liver tissue for 385, 357, 301, 245 and 217 days, respectively. We studied the possibility of mathematical description of the dynamics of analyte decomposition in a biomaterial (liver tissue) at the indicated temperatures using the hyperbolic equation. The coefficients in the hyperbola equation (kav), calculated according to the results of the experiment, for temperatures of -22 °C, 4 °C, 12 °C, 20 °C and 30 °C amounted to 6223, 3036, 2387, 1903 and 932, respectively., which is described by the equation: kav=101.19∙(50-to)-1272.78. It was established that on the basis of this equation it is possible to predict the nature of the stability of 2-MO-4-(2-P)HOB in the biomaterial (liver tissue) at temperatures in the range from -22 °C to 30 °C.

[Features of assay and decomposition dynamics of 2-methoxy-4-(1-propenyl)hydroxybenzene in biological material]. / Osobennosti opredeleniya i dinamiki razlozheniya 2-metoksi-4-(1-propenil)gidroksibenzola v biologicheskom materiale.

The objective was to study the features of assay and dynamics of decomposition of 2-methoxy-4-(1-propenyl)hydroxybenzene in biological material. Extraction, semi-preparation chromatography, TLC, HPLC, GC-MS and UV-spectrophotometry were used as test methods. 2-Methoxy-4-(1-propenyl)hydroxybenzene was extracted from the biological material by double infusion (45 min each) with ethyl acetate at a 2:1 mass ratio of isolating agent and biomatrix. Purification was performed by extraction and chromatography in a semi-preparative (190×10 mm) L 40/100 µm silica gel column using a hexane-dioxane (7:3) eluent. The analyte was determined by TLC methods (Sorbfil plates, hexane-acetone 9:1 as a mobile phase), HPLC [Discovery C18 HPLC Column (250×4.6 mm), acetonitrile-acetate buffer pH 5.5 (5:5) as a mobile phase], GC-MS [DB-5MS EVIDEX (25 m×0.2 mm) column with 5%-phenyl-95% dimethyl polysiloxane as a stationary phase], UV-spectrophotometry (95% ethanol as a solvent). The proposed assay method for 2-methoxy-4-(1-propenyl)hydroxybenzene in biomaterial (liver tissue) is validated for linearity, selectivity, accuracy and precision. The study results showed that the decomposition rate of the analyte increases as the store temperature increases. At 0-2 °C, 8-10 °C and 18-22 °C 2-methoxy-4-(1-propenyl)hydroxybenzene is stable for 480, 390 and 260 days respectively.

[Development of methods for determining and studying the persistence of 2,4-dimethylhydroxybenzene and 2,6-dimethylhydroxybenzene in biological material]. / Razrabotka metodik opredeleniya i izuchenie sokhranyaemosti 2,4-dimetilgidroksibenzola i 2,6-dimetilgidroksibenzola v biologicheskom materiale.

OBJECTIVE: To study the features of the determination and preservation of 2.4-dimethylhydroxybenzene and 2.6-dimethylhydroxybenzene in biological material. Extraction, semi-preparative chromatography, TLC, GC-MS and UV spectrophotometry are considered as methods of analysis. The 2.4- and 2.6-dimethylhydroxybenzenes were isolated from the biomaterial by double infusion (30 minutes each) with a mixture of ethyl acetate-acetone (7: 3) at a weight ratio of the insulating liquid and biomaterial of 2:1. Purification was carried out by extraction and chromatography in a semi-preparative (190×10 mm) column of silica gel L 40/100 µm using the eluent hexane-dioxane-propanol-2 (80: 5: 1). Analytes were determined by TLC (Sorbfil plates, mobile phase hexane-dioxane-propanol-2 (120: 5: 1)), GC-MS (DB-5MS EVIDEX column (25 m × 0.2 mm) with a stationary phase (5%-phenyl) - methylpolysiloxane), UV spectrophotometry (solvent - 95% ethanol). The developed methods for the determination of 2.4- and 2.6-dimethyl derivatives of hydroxybenzene in biomaterial (liver tissue) are validated according to the criteria of linearity, selectivity, correctness and precision. The study of the dynamics of decomposition of 2.4- and 2.6-dimethyl hydroxybenzene derivatives in model mixtures with liver tissue, carried out using the developed techniques showed that with an increase in temperature the duration of preservation of analytes in biological material decreases. Moreover, the 2.4-isomer is more stable during storage than the 2.6-isomer. At temperatures of -25 °C, 0-2 °C, 8-10 °C, 20-22 °C, 36 °C the duration of retention of 2.4-dimethylhydroxybenzene is 402, 379, 358 and 224 days, respectively, the duration of retention of 2.6-dimethylhydroxybenzene is 356, 312, 224 and 136 days, respectively.

[Determination of thiabendazole in the conditions of chemical and toxicological analysis of biomaterial]. / Opredelenie tiabendazola v usloviyakh khimiko-toksikologicheskogo analiza biomateriala.

OBJECTIVE: Is to study the features and to develop the methods for the determination of thiabendazole in the tissues of cadaveric organs and blood. When performing the experiments the methods of TLC, GC-MS and spectrophotometry were used. The advantages were substantiated and the optimal conditions for the release of thiabendazole from the tissues of organs and blood with acetone were determined. A variant of purification of the substance extracted from biomatrixes by the method of column chromatography of normal pressure (sorbent L 40/100 µm, mobile phase acetone-dichloromethane (9.5: 0.5)) is proposed. To identify the analyte by TLC the Sorbfil plates were used and a toluene-acetonitrile mobile phase (2:8). When identifying thiabendazole by a combination of gas-liquid chromatography and mass spectrometry (fragmentation of molecules by electron impact 70 eV) an HP-5MS column 30 m × 0.25 mm with a non-polar stationary phase (5% -phenyl) -methylpolysiloxane was proposed. The expediency of the spectrophotometric determination of thiabendazole on the basis of absorption in an acetonitrile medium has been shown. Methods for the determination of thiabendazole in tissues of organs and blood have been developed and validated. It is shown that the techniques meet the requirements of linearity, selectivity, correctness, precision and stability. The limits of detection of thiabendazole in the liver and blood are 0.14 and 0.10 mg, respectively; the limits of quantitative determination are 0.26 and 0.18 mg per 100 g of biomatrix.

[Forensic chemical study of Amlodipine]. / Sudebno-khimicheskoe issledovanie amlodipina.

THE AIM OF THE STUDY: Is to develop a method for determining amlodipine in the tissues of organs and blood, applicable in the practice of forensic chemical analysis. TLC, normal pressure column chromatography, HPLC and GC-MS were considered as methods of analysis. Amlodipine was isolated from the biomaterial by insisting twice with acetone for 30 min using a 2: 1 mass-isolating and biomatrix agent. The purification of recovered analyte was done in a column (150×10 mm) of a 30 µm Silasorb S-18 sorbent, eluting with an acetone - water solvent mixture (8:2). Preliminary identification was carried out in a thin layer of sorbent on «Sorbfil¼ plates, which was confirmed by HPLC and GC-MS methods. Determination by GC-MS was carried out in a column with a stationary phase of 5% phenyl-95% dimethylpolysiloxane. The fragmentation of molecules was an electron impact with an energy of 70 eV. Methods for the determination of amlodipine using GC-MS in biomatrix have been developed, which meet the criteria of linearity, selectivity, correctness, precision and stability. The limits of detection and quantitative determination of amlodipine in organ tissues (liver) are 0.14 and 0.24 µg/g, in blood - 0.12 and 0.20 µg/g, respectively. The methods were applied in the examination of a case of amlodipine poisoning and made it possible to determine the analyte in some organs and blood of the corpse.

[Features of determination of 2-methoxyhydroxybenzene in the study of biological material]. / Osobennosti opredeleniya 2-metoksigidroksibenzola pri issledovanii biologicheskogo materiala.

The aim of the study was to develop a method for the determination of 2-methoxyhydroxybenzene in biological material. TLC, UV spectrophotometry, HPLC and GC-MS were used in the experiments. The use of a mixture of ethyl acetate-acetone (7:3 by volume) for the isolation of 2-methoxyhydroxybenzene from biological material is justified. Optimal isolation conditions are established. Purification of the substance was carried out by extraction and chromatography in sorbent column (KCC-3) 80/120 µm. For preliminary identification, TLC was used on Sorbfil PTSX-AF-A-UV plates. Confirmation of identification was carried out by the UV spectrum in ethanol by HPLC with the retention time in a 250×4.6 mm column «SunFire C18¼ (mobile phase acetonitrile-0.025 M potassium dihydrogen phosphate solution 6: 4). Confirmation identification and quantification was performed by GC-MS using a fixed phase capillary column of 5% phenyl-95% methyl polysiloxane after derivatization of the analyte with N-trimethylsilyl-N-methyl trifluoroacetamide (heating for 30 min at a temperature of 60 °C). Ions 45, 58, 73, 91, 107, 136, 151, 166, 181, 196 m/z are present in the mass spectrum of the derivative. The validation of the methodology for the determination of 2-methoxyhydroxybenzene in biomaterial based on the application of the GC-MS method was carried out. The compliance of the methodology with the criteria of linearity, selectivity, correctness, precision and stability is established. The detection limit and the limit of quantification are 8 and 15 µg per 100 g of biomaterial, respectively.

[Felodipine distribution in organisms of warm-blooded animals]. / Raspredelenie felodipina v organizme teplokrovnykh zhivotnykh.

The objective of the work was to study felodipine distribution in warm-blooded animals (rats). The methods of TLC, GC-MS, and UV spectrophotometry were used in the experiments. A lethal dose of felodipine (1.05 g/kg) preliminary suspended in water was introduced intragastric into test animals (male rats of the Wistar line). The analyzed compound was isolated from solid tissues and blood of the animals with acetone, purified by the solvent replacement, and by macrocolumn chromatography with the Silasorb S-18 sorbent of 30 µm and polar eluent, acetonitrile-water (7:3). The analyte was identified by chromatographic behavior in a thin sorbent layer, retention time, and a set of positive ions in its mass spectrum, as well as by the UV spectrum. The analyte was quantitatively detected in biological matrices using UV spectrophotometry. The method was validated by the criteria of linearity, selectivity, accuracy, precision, limits of detection, and quantitative determination. The predominant content of felodipine was detected in tissues of the stomach (312.303±25.980 µg/g), small intestine with its contents (93.235±12.310 µg/g), stomach contents (80.072±8.510 µg/g), and in the spleen (26.083±1.758 µg/g).

[Features of the determination of amlodipine in a biological material]. / Osobennosti opredeleniia amlodipina v biologicheskom materiale.

The purpose of the work is to determine the optimal conditions for isolating amlodipine, to purify it by the method of column chromatography and to develop a method for detecting it in biological material. TLC, GC-MS, low pressure column chromatography, and HPLC were used for analysis. We studied the comparative isolation of amlodipine from biological material using 13 isolating agents of organic nature, water, and aqueous solutions. The use of acetone as an insulating agent for the extraction of amlodipine from tissues of cadaver organs has been substantiated. The possibility of purification of the analyzed compound from the endogenous substances of the biomaterial is shown by the method of reversed phase chromatography in a column of the Silasorp S-18 sorbent of 30 µm. A technique has been developed for detecting amlodipine in the tissues of cadaveric organs (liver), which corresponds to the necessary parameters of linearity, selectivity, accuracy, precision and stability. The limits of detection and quantification of amlodipine by the proposed method are 0.25·10-6 and 4.0·10-6 g, respectively, in 1 g of the biomaterial.

[Investigations into the distribution of neohistamine methylsulfate in the organism of the warm blooded animals following its intragastric administration]. / Izuchenie raspredeleniia neostigmina metilsul'fata v organizme teplokrovnykh zhivotnykh posle vnutrizheludochnogo vvedeniia.

The objective - of the present study was to elucidate the specific features of the distribution of neohistamine methylsulfate (proserin) in the organism of the omnivorous warm blooded animals following its intragastric administration. The analytical methods included TLC, HPLC, and UV-spectrophotometry. Neohistamine methylsulfate was administered intrgastrically to the male Wistar rats at a dose equivalent to the triple LD50 dose. The substance of interest was extracted by acetone from the biological matrices of the dead animals and purified by sequential treatment with the relevant solvents and chromatography in a thin layer of the reverse-phase sorbent (C14-C15 bonded phase model) with the elution in the buffer solution (pH 1.98) - acetone (8:2) system. The compound of interest was identified based on the Rf values (obtained by TLC), retention time (in HPLC), and the spectral characteristics. The quantitative determination of the analyte in the biomatrices was performed with the use of UV spectrophotometry. The analytical methods were validated based on the criteria for linearity, selectivity, correctness, and precision as well as detection threshold and results of quantitation. The largest amount of the study compound were determined in the heart (365.2±33.94 mcg/g), spleen (288.6±24.97 mcg/g), kidney (127.6±9.33 mcg/g), and the gastric walls (124.6±12.17 mcg/g) of the experimental animals.

[The specific features of the distribution of 2,4- and 2,6-di--butylhydroxybenzenes on the body of the warm-blooded animals]. / Osobennosti raspredeleniia 2,4- i 2,6-di--butilgidroksibenzola v organizme teplokrovnykh zhivotnykh.

The present study was designed to elucidate the character of the distribution of 2,4- and 2,6-di-tret-butylhydroxybenzenes (2,4-DTBHOB and 2,6-DTBHOB respectively) in the body of the warm-blooded animals (rats) following the administration of the three-fold LD50 dose into the stomach. Both 2,4-DTBHOB and 2,6-DTBHOB were extracted from the blood and the organs of the perished animals by means of two-fold incubation of the sampled tissues in ethyl acetate with the subsequent purification of the isolates by passing the extracts through a L 40/100 mcm silicagel column using hexane:dioxane (8.5:1.5) for 2,4-DTBHOB and hexane:dioxane (97.5:2.5) for 2,6-DTBHOB as eluants. The compounds of interest were identified and quantified by means of TLC, HPLC, and UV-spectrometry. The study has shown that both 2,4-DTBHOB and 2,6-DTBHOB were present in the organs and blood of the poisoned animals in the unmetabolized form. Their largest amounts (mg/100 g) were found in the contents of the stomach, the small intestines with the contents and in the spleen.

[The peculiar features of the distribution of 2-metoxy-4-(1-propenyl)-hydroxybenzene in the organism of the warm-blooded animals]. / Osobennosti raspredeleniia 2-metoksi-4-(1-propenil)-gidroksibenzola v organizme teplokrovnykh zhivotnykh.

The present study was designed to elucidate the distribution patterns of 2-metoxy-4-(1-propenyl)-hydroxybenzene in the organism of the warm-blooded animals (rats) after its intragastric administration at a dose equivalent to three 50% lethal doses (LD-50) for this compound. 2-metoxy-4-(1-propenyl)-hydroxybenzene was extracted in the unmodified form from the organs and blood of the dead animals after the dualfold infusion of the tissues with ethyl-acetate and purification by chromatography on a macrocolumn with silica gel L 40/100 mcm making use of the hexane-acetone mixture (7:3) mobile phase as the eluent. TLC, HPLC, and UV-spectrometry were employed to identify and quantify the analyte. The study has demonstrated the presence of unmetabolized 2-metoxy-4-(1-propenyl)-hydroxybenzene in the organs and blood of the poisoned animals. The largest amounts of this compound (expressed in milligrams per 100 g of the tissue) were accumulated in the stomach with its contents (236.22±28.21), small intestine with their contents (122.29±15.55), lungs (44.28±2.10), and spleen (44.00±4.70).

[The distribution of 2-(dimethylamino)ethyl-(1-hydroxycyclopentyl)(phenyl)acetate in the organism of the warm-blooded animals after its intra-gastric administration]. / Raspredelenie 2-(dimetilamino)étil-(1-gidroksitsiklopentil)(fenil)atsetata v organizme teplokrovnykh zhivotnykh pri vnutrizheludochnom vvedenii.

The objective of the present study was to elucidate the distribution of 2-(dimethylamino)ethyl-(1-hydroxycyclopentyl)(phenyl)acetate in the organism of the warm-blooded animals after its intra-gastric administration. The methods applied in the study included thin layer chromatography in silicagel, aci-nitroprosalt staining reaction, UV-spectrophotometry,, and GC-mass spectrometry. The identification and the quantitation of 2-(dimethylamino)ethyl-(1-hydroxycyclopentyl)(phenyl)acetate in the organs and blood of the warm-blooded animals were carried out within 20, 150, and 360 min after a single intra-gastric administration of 1300 ml of this poisonous substance. It was shown that the largest amounts of 2-(dimethylamino)ethyl-(1-hydrpxycyclopentyl)(phenyl)acetate at the above time-points were present in the tissue of the stomach and small intestine, brain, muscles, spleen, and lungs of the animals.

[The peculiar features of the distribution of 2-(dimethylamino)ethyl- (1-hydroxycyclopentyl) (phenyl) acetate in the organism of warm-blooded animals after its intravenous administration]. / Osobennosti raspredeleniia 2-(dimetilamino)étil-(1-gidroksitsiklopentil)(fenil)atsetata v organizme teplokrovnykh zhivotnykh pri vnutrivennom vvedenii.

The objective of the present study was to elucidate the dynamics of the distribution of 2-(dimethylamino)ethyl-(1-hydroxycyclopentyl)(phenyl) acetate in the organism of warm-blooded animals (rats) after its intravenous administration to the animals. The identification and the quantitative determination of 2-(dimethylamino)ethyl-(1-hydroxycyclopentyl)(phenyl) acetate present in the organs and blood of the warm-blooded animals were carried out with the use of chromatography in a thin layer of silica gel, chromogenic reaction for the synthesis of the acinitro salt, UV spectrophotometry, and gas chromatography mass-spectrometry (GCh-MS). The quantitation was performed on days 5, 20, 150, and 360 minutes after the intravenous administration of 2-(dimethylamino)ethyl-(1-hydroxycyclopentyl)(phenyl) acetate to the rats. The maximum amounts of cyclopentolate were found in the spleen, brain, lungs, and heart of the experimental animals.

[The determination of 2,4-di-tret-butyl hydroxybenzene for the purpose of the chemical toxicological study of the biological materials]. / Opredelenie 2,4-di-tret-butilgidroksibenzola pri khimiko-toksikologicheskom issledovanii biologicheskogo materiala.

The objective of this work was to study peculiarities of identification of 2,4-di-tert-butyl hydroxybenzene (2,4-DTBHOB) in blood and the tissues of various organs with the use TLC, UR- and UV-spectrophotometry. The results of the study suggest the expediency of the application of ethylacetate as the extractive agent for the isolation of 2,4-DTBHOB from the biological materials. The optimal conditions for 2,4-DTBHOB extraction by this method were developed based on the decontamination of the analyte by means of removal of the organic substances of biological matrices using the L 40/100 mcm sorbent columns with the hexan/dioxane mixture (8.5:1.5) as the mobile phase. The method for the determination of 2,4-di-tert-butyl hydroxybenzene in the tissues of various organs (namely, liver) and blood has been developed. The proposed method allows to determine the minimal quantities of 2,4-DTBHOB present in the biological objects equivalent to 0.36 mg and 0.28 mg in the hepatic tissue and blood respectively.