Chemical-toxicological Analysis Research Articles

Fatal consequences caused by prolonged chloroform inhalation in a child

Introduction. Chloroform intoxication as a result of inhalation is usually associated with occupational exposure. Fatal cases of accidental and intentional chloroform poisoning are extremely rare. The aim of this work was to report a case with fatal consequences caused by prolonged chloroform inhalation in a child. Case outline. We report a case of a three-month-old child found dead by its mother in their home. Investigation provided the data about two refrigerators in the house, which were not entirely functional, and were filled with a refrigerant based on chloroform, and about a recent house spraying with a pesticide also based on chloroform. Forensic autopsy was performed the following day. Autopsy established the existence of malnutrition, dehydration, brain and lungs edema, the presence of very scarce contents in the digestive tract, and the enlargement of the abdominal lymph nodes. The initial stage of liver degeneration was noted on histopathological examination. Chemical-toxicological analysis of organ tissue samples (brain, lungs, spleen, liver with gall bladder, kidney and bladder, stomach, small and large intestine) performed using the techniques of headspace gas chromatography with mass detector, confirmed chloroform poisoning. Conclusion. The emaciation underlying the dysfunction of organ systems provided a grim frame for a child to succumb to chloroform toxicity. The proper use and maintenance of domestic appliances, and careful application of chemical agents indoors is an imperative, especially in the vicinity of children. Low levels of chloroform inhaled from the room air may have fatal consequences in a susceptible individual.

The investigations of propranolol by HPLC method suitable for a chemical-toxicological analysis

Topicality. Therapeutic monitoring when using propranolol hydrochloride, analysis of the drug in dosage forms and biological objects, identification and quantitative determination of the drug during intoxication are carried out using sensitive and selective methods. Among the modern methods of analysis for creating a database of parameters of identification and quantitative determination of analytes arrays in biological objects HPLC method is one of the most suitable methods with high sensitivity and selectivity.Propranolol hydrochloride (anaprilin) - (±)1-isopropylamino-3-(1-naphthyloxy) -2-propanol hydrochloride – non-selective β-adrenoceptor blocker, which is characterized by antianginal, antihypertensive and antiarrhythmic effects and is used for treatment of coronary heart disease, heart rhythm disorders and some forms of hypertension. The previously developed HPLC methods of propranolol analysis are based on the application of various chromatographic conditions (mobile phase composition, isocratic or gradient elution, detecting at one or several wavelengths, selection of sensitive and selective detector) due to individual properties of a substance. Taking into account the possibility of complex treatment of diseases of the cardiovascular system with the use of different drugs, the analysis by a unified HPLC methodology is an actual task of the study.The purpose of this work is identification and quantitative determination of propranolol hydrochloride by a unified HPLC methodology, which allows obtaining reliable and reproducible research results that are suitable for drug analysis in biological objects.Materials and methods of research. Chromatography of the investigated substance was performed on a microcolonial liquid chromatograph "Milichrome A-02" ("EcoNova", Novosibirsk, Russia) in an reverse-phase variant using a metal column with a nonpolar sorbent Prontosil 120-5C 18 AQ, 5 μm. For elution of the drug were used a mixture of solvents - acetonitrile with 0,2 M solution of lithium perchlorate in 0,005 M solution of acid perchloric. The linear gradient from eluent A (5% acetonitrile and 95% buffer solution) to eluent B (100% acetonitrile) for 40 minutes created conditions for the exit from the column of all component parts of the sample as narrow zones. The flow rate of the mobile phase has been formed 100 μl/min, column temperature – 37 - 40 °С; pump pressure – 2,8 – 3,2 MPa; injection volume – 4 μl. Multi-channel detection of a substance was performed by a UV detector in 8 wavelengths: 210, 220, 230, 240, 250, 260, 280 and 300 nm. Results and their discussion. In carrying out identification of propranolol were established absolute parameters of retention time (19,40-19,54 min) and retention volume (1940,8-1955,2 μl), spectral relationships, detection limit of the substance in the sample (4,0 μg / ml or 16,0 ng in the sample), the values of the coefficients of the symmetry of the peaks of the substance (0,94-1,10) and the coefficients of capacity ratio (11,94-12,04).The regression coefficients of the calibration graph, which corresponds to the equation of the straight line S = 0,00565 С were calculated by the least squares method. The correlation coefficient was equal to 0,9987. Validation characteristics of HPLC-method for determination of propranolol: linearity range (5,0-100,0 μg / ml), limit of quantitative determination (5,0 μg / ml or 20 ng in the sample), correctness and accuracy on the basis of the results of the quantitative determination of the preparation by the HPLC method in model solutions were calculated. It was established that the relative uncertainty of the average result did not exceed ± 2,11% when using the proposed method of HPLC analysis of propranolol hydrochloride in model solutions.Conclusions. Identification and quantitative determination of propranolol hydrochloride with the use of a unified HPLC method suitable for a chemical toxicological study was carried out.

The choice of the conditions for the preparation of the pregabalin samples from the biological fluids with the use of the liquid-liquid and solid phase extraction techniques

The objective of the present study was the development of the methods for the isolation and identification of pregabalin for the purpose of chemical toxicological analysis (CTA). The authors describe the methods used to obtain pregabalin from the model mixtures of urine and blood plasma with the use of liquid-liquid and solid phase extraction. In addition, a method for the quantitative determination of pregabalin by means of combined gas chromatography mass-spectrometry was applied.

The choice of the conditions for the preparation of the pregabalin samples from the biological fluids with the use of the liquid-liquid and solid phase extraction techniques

The objective of the present study was the development of the methods for the isolation and identification of pregabalin for the purpose of chemical toxicological analysis (CTA). The authors describe the methods used to obtain pregabalin from the model mixtures of urine and blood plasma with the use of liquid-liquid and solid phase extraction. In addition, a method for the quantitative determination of pregabalin by means of combined gas chromatography mass-spectrometry was applied.

РАЗРАБОТКА МЕТОДИКИ ИЗОЛИРОВАНИЯ ТОФИЗОПАМА В МОДЕЛЬНОЙ СМЕСИ МОЧИ

Forensic chemical examination is carried out in order to isolate, identify and quantify toxic, narcotic, psychotropic and potent substances in the organs and fluids of the human body. The present study we researched the process of extraction of 2,3-benzodiazepine - tofisopam. There have been cases of tofisopam poisoning. And there are no descriptions of tofisopam isolation from biological fluids in the literature. Liquid extraction, an effective and commonly used method of isolation in the chemical-toxicological analysis, is used when extracting substances from blood, lymph, saliva, urine and stomach washings. The process of isolation may be influenced by the nature of the organic solvent, pH, the presence of an electrolyte, time and frequency of extraction. We have studied the effect of each factor on tofisopam isolation from aqueous solutions. It has been found that the optimal organic solvent for the extraction of the solutions is dichloroethane, which extracts maximum amount of the analyte at pH = 5.0. Saturated sodium sulphate has a salting-in effect for tofisopam. The optimum conditions for tofisopam isolating are 7 minutes with double extraction. Based on the research method of tofisopam isolating the model mixture of urine was developed. We found that this model urine mixture isolates 66.51-67.9l % of tofisopam. We performed validation assessment of the developed method for evaluation of precision and accuracy. The assessment showed the suitability of techniques for the analysis.

Pressurized planar electrochromatography as a supporting tool for qualitative toxicological chemical analysis with thin-layer chromatography and UV–Vis spectrometry

ABSTRACTPressurized planar electrochromatography (PPEC) was applied to support qualitative toxicological chemical analysis performed with thin-layer chromatography (TLC) and UV–Vis spectrometry. Based on retention/migration distance data of substances obtained in TLC and PPEC systems and database of their wavelength maxima of remission UV–Vis spectra as well, a combined fit factor was calculated for substance identification. The involvement of PPEC, TLC, and UV–Vis spectral data together in calculation of the combined fit factor lead to its lower values for substances, which were not identical with reference, in comparison with those when the combined fit factor was calculated using TLC and spectral data only. The results evidence that involvement of PPEC data in qualitative toxicological chemical analysis performed with TLC and UV–Vis spectrometry enhances reliability of it.

Toxicological Chemical Analysis of Methanol in Blood of Patients with Acute Ethanol Intoxication for Determining Detectable Quantities of Methanol and Analysis of the Correlation Between Ingested Alcohol

Summary The aim of the study was to carry out a toxicological chemical analysis of methanol in detectable quantities in the blood of patients with acute alcohol intoxication. Blood samples from 85 patients with acute alcohol intoxication were analysed for the presence of methanol. All patients with acute methanol intoxication were excluded from the study. The methods of gas chromatography with vapor-phase analysis (head-space) and flame ionization detection (FID) were used. The limit of detection (LOD=0.015 g/L) and the limit of quantification (LOQ=0.025 g/L) of methanol in whole blood were evaluated. In 30% of the cases, methanol was found in the blood in detectable quantities. The levels of methanol were on the average 5 to 6 times lower than the toxic methanol level (0200 g/L) and they were not due to natural metabolic processes (ingestion of fruit, fruit juices or vegetables). No reliable statistically linear correlation between the concentration of ethanol and methanol was found. Methanol subintoxications are major factors in alcohol intoxications, in which the quantity of the alcohol ingested is not as important as its quality. Chronic methanol subintoxication of people who often consume alcohol of poor quality is discussed.

The chemical toxicological analysis of sertindole

Sertindole is an "non-typical" neuroleptic extensively used for the treatment of schizophrenic patients. The detection of intoxication with this medication implies the necessity of development of the optimal methods for its isolation from the biological materials and further identification. The objective of the present work was to study the influence of various factors on the efficiency of sertindole extraction from solutions, the elaboration of the methods for its isolation from biological objects, detection, and quantitative determination in the extracts from these objects. Investigations into the influence of various factors on the isolation of sertindole from solutions included characteristic of the chemical nature of the organic solvent and the electrolyte, measurements of pH, time and frequency of extraction with the use of UV spectrophotometry. Isolation of sertindole from the liver, kidneys, brain, heart, gastric and intestinal contents was carried out by the method of A.A. Vasil'ev. Moreover, we have developed an original method for the detection of sertindole in the extracts using TLC, UV spectrophotometry, and HPLC. The qualitative determination of sertindole in the extracts from the internal organs, blood plasma, and urine was performed by HPLC. The optimal conditions for sertindole liberation from the extracts have been found and TLC-screening conditions proposed. The TLC, UV spectrophotometric, and HPLC techniques specially modified for the determination of sertindole in the extracts were used. It was shown that the maximum amounts of sertindole were present in the liver and brain within 24 hours after acute poisoning. In the kidneys, stomach, and intestines, it accumulated in smaller quantities Extracts from the heart did not contain sertindole. Maximum efficiency of the sertindole extraction during 24 hours was achived from blood plasma.

Seventy Years of Biochemical Subjects' Development in Pharmacy Curricula: Experience from Serbia.

SummaryIntroductionThe pharmacists played an important role in the development of biochemistry as applied chemistry in Serbia. What is more, the first seven state chemists in Serbia were pharmacists. State chemists performed the chemical-toxicological analysis as well as some medical and biochemical ones. When it comes to the education of medical biochemists as health workers, the period after the beginning of the second half of the twentieth century should be taken into account because that is when the training of pharmaceutical staff of the Faculty of Pharmacy, University of Belgrade, begins on the territory of Serbia. This paper presents the development of medical biochemistry through the development of curriculum, personnel and literature since the foundation of the Faculty of Pharmacy in Serbia until today.ObjectiveThe aim of this paper is to present the historical development of biochemistry at the Faculty of Pharmacy, University of Belgrade, through analysis of three indicators: undergraduate and postgraduate education of medical biochemists, teaching literature and professional associations and trade associations.MethodThe method of direct data was applied in this paper. Also, desktop analysis was used for analyzing of secondary data, regulations, curricula, documents and bibliographic material. Desktop research was conducted and based on the following sources: Archives of the University of Belgrade-Faculty of Pharmacy, Museum of the History of Pharmacy at the University of Belgrade-Faculty of Pharmacy, the Society of Medical Biochemists of Serbia and the Serbian Chamber of Biochemists.Results and conclusionThe curricula, the Bologna process of improving education, the expansion of the range of subjects, the number of students, professional literature for teaching biochemistry, as well as professional associations and trade associations are presented through the results.

Chemical analysis of wastewater as a new way of monitoring drugs and medicines consumption at workplace

The available information on the quality and frequency of illegal psychoactive substances used or medicines misused by workers, are often out of date at the time of its publication. This is due to the dynamic introduction of new synthetic drugs on the black market, changes in trends in the recreational use of medicines and the lack of readily available and reliable tests for fast identification. Strategy for detection of narcotic and non-medical psychoactive drugs use at workplace should embrace all possible sources of information. Classical sources of information on the use of psychoactive substances at the workplace include: statistical data (general information on trends and magnitude of drug and medicine addiction collected by the Polish National Police, the National Bureau for Drug Prevention and emergency medical services), surveys, psychomotor tests and qualitative and quantitative analyses of biological material. Of the new and promising methods, used throughout the world in recent years, chemical-toxicological analysis of surface water and wastewater deserve special mention. An increasing interest in the study of urban waste water can significantly complement the source of knowledge about drug and medicine addiction using obtainable conventional methods. In recent years, a municipal wastewater analysis has become a new and very promising way of collecting updated information on the use of psychoactive substances and medicines. It seems that this kind of study may play an important role in the ongoing monitoring of drug and/or medicines use by selected groups of population (e.g., students, military, firemen, policemen, etc.).

Chromatography as Method for Analytical Confirmation of Paracetamol in Postmortem Material Together with Psychoactive Substances.

Introduction:Paracetamol (Acetaminophen) in addition to aspirin is the most commonly used analgesic and antipyretic medication by millions of patients worldwide. It is an example that paracetamol as medicine that in the world is provided without a doctor’s prescription, can lead to death. Today paracetamol became an integral part of a heroin mixture and is very popular at the street market. The main reason for this is that it can be obtained without a prescription, it is cheap, and by most people well tolerated without side effects. It is probably used for “cutting” the pure heroin, as it says in the jargon, and in that manner from small amount of pure drug is obtained greater amount, which is then sold on the street. The goal is to identify presence of paracetamol, by analytical method of gas chromatography mass spectrometer (GC-MS) in postmortem material together with psychoactive substances.Material and methods:For chemical-toxicological analysis is used biological material collected trough autopsy of 20 deceased people, suspected to have died due to psychoactive substance overdose. All received samples are stored at -20 ° C until analysis at our laboratory. From processed 47 samples that were analyzed in the period from 2014 to 2015, 19 are blood samples, urine 19, 3 samples of stomach contents, and 6 samples of bile content. Deceased were middle-aged, of which only 7 were female. The tested samples were processed according to two methods of extraction. Extraction by XAD-2 resin, and the extraction by the method of salting out with sodium tungstate. Extracts of the samples were then dissolved in chloroform and continued analysis at the analytical instrument. Identification of the paracetamol presence, in the test biological samples is demonstrated by the technique of gas chromatography with mass spectometry (hereinafter referred to as GC-MS). The technique of GC-MS is a selective, sensitive and reliable, and is therefore considered a “gold standard” for determining the drug, and the drug substance. Used GC-MS instrument was an Agilent 7890A with helium as the carrier gas.Results:The analysis of blood samples, urine, bile and stomach contents, obtained after the autopsy of deceased persons, by using gas chromatography with mass spectrometry, in analytical manner confirmed the fact that paracetamol is a very common component of psychoactive substances poisoning. In our assay of samples we detected psychoactive substances (heroin, codeine, morphine, sertraline, diazepam), and almost all were found in the combination with paracetamol, indicating the poor quality of illicit drugs sold on the market.Discussion:Paracetamol (Acetaminophen) is a very common component in mixtures of street drugs. Such mixtures almost anyone can afford, but the very quality of these drugs has become extremely low, because it does not sell the pure substance, but is mixed with various medications. According to research Pantazia et al. the heroin mixture proportion of the heroin is very small so a lot of that mixture has only 3% of heroin, a large number of cases can be only 1% of pure heroin. Most of the time it replaces caffeine and paracetamol. According to the Risser et al. reason why acetaminophen component is present in these mixtures is because it can be purchased without a prescription, it is cheap, well tolerated by most people and shows no side effects.Conclusion:When we talk about illegal drugs, we must emphasize the fact that there is no quality control, or the composition of the drug. The composition of the drug purchased on the black market is still unknown to potential user. While reaching the final drug users it pass through many hands, and at each step something is added to increase earnings. Most often present additives or impurities in narcotic drugs that are added are caffeine, ephedrine, acetaminophen, acetylsalicylic acid (aspirin) and additives such as powders, cement and chalk.

Investigations of the distribution of aripiprazole in the internal organs and biological fluids of the laboratory animals in case of acute intoxication

Despite the present-day extensive application of aripiprazole, there are many cases of its overdose and of poisoning with this compound. The objective of the present study was to detect and quantify aripiprazole in the internal organs and biological fluids of the laboratory animals in case of acute intoxication. The experiments were carried out on white mice of both sexes weighing 20.5 and 25.7 g. Aripiprazole was isolated from the liver, kidneys, brain, and heart as described by A.A. Vasil'eva and from the plasma and urine by the newly developed original methods. Aripiprazole was identified and quantitatively determined in the extracts from the aforementioned organs and tissues with the use of HPLC. The data obtained on the completeness of extraction from the liver, kidneys , and brain of the laboratory animals indicate that aripiprazole accumulated in the highest concentrations in the brain and kidneys within 24 hours after acute poisoning. Ist content was significantly lower in the liver while no traces of aripiprazole were found in the heart of the mice. The methods for aripiprazole isolation from the urine and blood plasma are described. The maximum amounts of aripiprazole were detected in blood plasma within 24 hours after acute intoxication. It is concluded that the proposed methods for aripiprazole isolation from the biological fluids (blood plasma and urine) can be included in the scheme of the chemical toxicological analysis of this compound.

Application of two-dimensional high-performance thin-layer chromatography to qualitative and quantitative toxicological-chemical anal

The present paper describes various application possibilities of high-performance thin-layer chromatography (HPTLC) for qualitative and quantitative toxicological-chemical analysis. Exemplified by 115 toxicological relevant drugs, a simple and fast two-dimensional HPTLC procedure is presented, suited for the undirected qualitative toxicological-chemical analysis. Here, we demonstrate that the separation performance can be increased significantly by identifying substances on the basis of the two migration distances together with the remission spectra maxima, measured with a HPTLC scanner (densitometer). The values calculated for the discrimination power and the identification power were found to be comparable with those of other chromatographic procedures, commonly used for toxicological-chemical analysis (high-performance liquid chromatography [HPLC], gas chromatography-mass spectrometry [GC-MS], and liquid chromatography-mass spectrometry [LC-MS]). While a scanner increases clearly the efficiency of qual...

Schwere Enzephalopathie nach Einnahme eines „Phytopharmakons“ aus Vietnam

A 59-year-old woman went into coma after she had taken a phytopharmacon from Vietnamese generally used as an antidiabetic drug to treat her skin disease. CT-scans revealed signs of pneumonia and cerebral edema. Severe brain damage was diagnosed by MRI-investigation. By chemical-toxicological analysis of the drug glibenclamide was identified in a concentration of 1.1 mg/g. The patient developed severe irreversible encephalopathy. By neurorehabilitative treatment her physical status slightly improved, but she died after 13 months without regaining consciousness. The cause of losing consciousness remained unclear, however, severe hypoglycaemia following the use of the drug may be taken into account. An urgent warning against the use of such preparations is highly recommended.

Medicolegal characteristics of homicides in Belgrade population

OBJECTIVE. Homicide is a destruction of human life, and it essentially conditioned by socio-economic situation in the society. The aim of this study is to analyze the frequency and other significant epidemiological and medicolegal characteristics of homicides in the population of Belgrade. METHODS. An analysis was performed of all homicide cases in which autopsies were performed at the Institute of Forensic Medicine in Belgrade from 2003. to 2005. Data were obtained by using the autopsy records, the investigation reports, the heteroanamnesis obtained from family members of the fatally injured persons and the results of chemical toxicological analysis. RESULTS. There were a total of 143 cases of autopsies of homicide victims. The majority of victims were males (103 or 72.03%) aged from 21 to 30 (25.17%). Homicides were mostly performed by using mechanical weapons only (127 or 88.8%). In most of the cases five or more injuries were registered per victim (48 victims or 33.57%) or only one injury (52 or 36.36%). Most of entrance wounds were located on the anterior side of the body. CONCLUSION. We demonstrated a gradual decrease in the number of murders in our population, and therefore we can expect a decrease in the absolute number of homicides in the future. Keywords homicide; male; firearms; multiple trauma; forensic medicine Language: sr