The determination of phoxim in cadaveric material by gas-liquid chromatography]

The developed gas-liquid chromatographic procedure for forensic chemical detection and measurement of phoxim in cadaveric material permits the detection in 25 g of an organ of 44 to 52% of added phoxim. The threshold of phoxim measurement in 100 g of the liver is 0.04 mg, the least volume of phoxim detectable being 0.02 g. The developed gas-liquid chromatographic technique should be used as an additional method together with thin-layer chromatography, for a more objective evaluation of the results of forensic chemical analysis of cadaveric material for phoxim.     

An evaluation of methods for isolating antiparkinson preparations from cadaveric material

Methods of amedine, amyzyl, and tropacine isolation from cadaveric material, blood and urine were developed. They ensure higher output of the given substances as compared with conventional methods of isolation of toxicologically significant substances. An extraction-photometric method was developed for estimation of amedine, amyzyl, and tropacine in the cadaveric material.     

The detection of novocaine and p-aminobenzoic acid in cadaveric material

Microcrystalloscopic reactions, TLC and UV spectroscopy methods for novocainum and p-aminobenzoic acid identification in medicolegal examination of the cadaveric material were developed. Sensitivity and specificity of microcrystalloscopic reactions were studied.     

The detection of the presence of azafen in cadaveric material

Possibility of isolating azaphen from the cadaveric material by acidified water and acetonitrile (as extractant) is shown. Isolation rate (75.6%) of azaphen (with 1 mg of preparation added to 25 g of the liver by acetonitrile is significantly higher than in isolation by acidified water (41.7%).     

The gas chromatographic detection of acetylene in cadaveric material]

Acetylene traces were detected by gas chromatography in the cadaveric right crural muscle of a 30-year-old man dead from an explosion of an acetylene reservoir at a plant. Acetylene was identified using the absolute calibration method on 3 standard gas chromatographic columns, reaction gas chromatography, and acetylene "deduction" by silver sulfate on silicagel.     

Capillary gas-liquid chromatography separation of phenethylamines in amphetamine-positive urine samples

Good gas chromatography (GC) separation of molecules is essential for clean gas chromatography/mass spectrometry (GC/MS) confirmation of compounds. The trifluoro derivatives of ephedrine (E) and methamphetamine (MA) coelute on dimethyl silicone capillary columns, such as DB-1, which are most commonly used by chromatographers. Methods are described to separate E and MA to aid GC/MS confirmations of methamphetamine, ephedrine, or both E and MA together, whichever may be present in Enzyme Immunoassay (EIA)-analyzed amphetamine-positive urine samples. The use of the heptafluoro derivatives of E and MA on a DB-1 column, or the trifluoro derivatives of E and MA on a DB-17 column, is suggested for good gas chromatographic separation.     

The use of high-pressure liquid chromatography for identifying barbiturates in cadaveric material]

A method for chemical toxic analysis of barbiturates has been developed, making use of acetone as an extracting agent and high-pressure liquid chromatography for the identification of the isolated substances. Analysis with the use of this method is preceded by extraction and chromatographic purification. The co-extractive substances do not interfere with the identification of barbiturates.     

The analysis of tiapride in cadaveric material

To optimize conditions of tiapride isolation from cadaveric organs, we compared the results of conventional methods by Stas-Otto, A.A. Vasilyeva and V.F. Kramarenko which provide tiapride isolation up to 50% and a new precise and reproducible method providing 60 +/- 2% tiapride isolation. Identification of tiapride isolated from cadaveric material was made with thin-layer chromatography and high performance liquid chromatography. The latter assay employed the method of external standard. The original techniques proposed identify and measure tiapride in hepatic samples in the presence of unidentified endogenic compounds. The techniques are rapid, selective, sensitive and reproducible.     

The determination of chromium in cadaveric material by using cyclohexanecarboxylic acid

Method of chrome detection in the course of forensic chemical investigation in the cadaveric material on the basis of cyclohexan-carbonic acid use is presented. Results of experimental researches showed efficacy of method tested as compared to the common one. Method suggested can be used in laboratory conditions to extract chrome from visceral organs of human cadaver.     

The use of gel chromatography for the purification of beta-adrenoblockaders isolated from cadaveric material]

Efficacy of gel chromatography for purification of extracts from cadaveric material containing beta-adrenoblockers was shown in model tests. Distribution curves and chromatographic features of beta-adrenoblockers obtained on hydrophilic and lipophilic-hydrophilic Sephadex were studied.     

The detection of isoniazide in the cadaveric blood and plasma by high performance liquid chromatography with a diode matrix detector

The authors describe the analytical procedure for the rapid detection of isoniazide in the cadaveric blood and plasma using high performance liquid chromatography with a diode matrix detector (HPLC-DAD). The method is designed for toxicological and forensic medical analyses. The preliminary preparation of the samples includes protein precipitation with trichloroacetic acid, formation of isoniazide derivatives with cinnamic aldehyde, and chromatographic analysis on an Eclipse XDB-C18 column with registration of absorption at a wavelength of 340 nm. The mobile phase is a mixture of methanol and 0.05 M ammonium acetate buffer (50:50 v/v), pH 3.8. The detection limit is 0.5 mcg/ml in plasma and 1 mcg/ml in blood hemolizate. The qualitative determination is possible in a concentration range from 2 to 200 mcg/ml. Mean square deviation does not exceed 12% in a concentration interval from 2 to 50 mcg/ml.     

The gas chromatographic determination of carbophos in cadaveric material

The authors developed a method of malathion insecticide determination in the cadaveric material (blood and wall of the stomach) including extraction of 5 ml of blood (5 g of fragmented tissue of stomach wall) by hexan; preparative chromatographic purification of extract on silicagel layer L 5/40 mkm in hexan-diethyl ether system 10:2; Gas-liquid chromatographic investigation on column with 5% SE-30 and 5% XE-60 (Chromatograph "Colour-106" with thermionic detector). This method makes it possible to detect 72-76% of malathion added.     

The retention of alkyldinitrophenol compounds in cadaveric material]

The preservation of alkyl dinitrophenol compounds in corpse liver tissue was under study. The content of these compounds was assessed after various periods of the corpse storage.     

Preservation of methanol in cadaveric material

Duration of preservation of methanol in cadaveric material at 20 +/- 3 degrees C during 4-13 months was studied on 19 model and expert objects of cadaveric material (muscle tissue, kidney, blood, urine). Exponential relationship between methanol concentration and duration of storage of the object was detected. Methanol concentration decreased by 30-70% during the first weeks, after which the process decelerated to 5-10% a month. Toxicologically significant concentrations of endogenous methanol were not revealed in any case.     

Determination of trasodone in cadaveric material

Methods of trasodone isolation from cadaveric material by water and acetonitrile at pH-2.0, which may be used in expert practice, were developed. Acetonitrile method is recommended for everyday practice as it allows one to isolate about 60% of trasodone and to obtain extracts with lower content of extractive substances. Detection limit in case of trasodone isolation by acidified water is 50 micrograms in 25 g of the liver and by acetonitrile--25 micrograms in 25 g of the liver and kidney.     

The isolation of amitriptyline from cadaveric material using acetonitrile

Method of amitriptyline isolation from the cadaveric material using acetonitrile as extractant is suggested. This method makes it possible to extract in average 76.09% of substance previously added in quantity of 1 mg to 25 g of the liver. Method was successfully used in analysis of expert material.     

尿中吗啡的氮磷检测——气相色谱分析法

目的建立尿中吗啡的简便快速、灵敏可靠的GC/NPD分析方法。方法样品尿加内标烯丙吗啡,酶或酸催化水解,氯仿-异丙醇(9:1)液液提取或GDX403树脂固相提取,BSA衍生化,HP-5柱和氮磷检测器进行分析。结果 提取率62％～85％,检出限1.2～3.1ng/ml,线性范围20～2000ng/ml,回收率(97％～99％)±(6％~9％)(Mean±cv,N=5)。结论 方法适合于实际案件中尿样的检验。