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1.
BMC Public Health ; 24(1): 2325, 2024 Aug 27.
Artigo em Inglês | MEDLINE | ID: mdl-39192313

RESUMO

BACKGROUND: In recent years, overdoses involving illicit cocaine, methamphetamine, and other stimulants have increased in the U.S. The unintentional consumption of stimulants containing illicit fentanyl is a major risk factor for overdoses, particularly in Massachusetts and Rhode Island. Understanding the drug use patterns and strategies used by people who use stimulants (PWUS) to prevent overdose is necessary to identify risk and protective factors for stimulant and opioid-involved overdoses. Mixed-methods research with people who distribute drugs (PWDD) can also provide critical information into the mechanisms through which fentanyl may enter the stimulant supply, and the testing of drug samples can further triangulate PWUS and PWDD perspectives regarding the potency and adulteration of the drug supply. These epidemiological methods can inform collaborative intervention development efforts with community leaders to identify feasible, acceptable, and scalable strategies to prevent fatal and non-fatal overdoses in high-risk communities. METHODS: Our overall objective is to reduce stimulant and opioid-involved overdoses in regions disproportionately affected by the overdose epidemic. To meet this long-term objective, we employ a multi-pronged approach to identify risk and protective factors for unintentional stimulant and opioid-involved overdoses among PWUS and use these findings to develop a package of locally tailored intervention strategies that can be swiftly implemented to prevent overdoses. Specifically, this study aims to [1] Carry out mixed-methods research with incarcerated and non-incarcerated people who use or distribute illicit stimulants to identify risk and protective factors for stimulant and opioid-involved overdoses; [2] Conduct drug checking to examine the presence and relative quantity of fentanyl and other adulterants in the stimulant supply; and [3] Convene a series of working groups with community stakeholders involved in primary and secondary overdose prevention in Massachusetts and Rhode Island to contextualize our mixed-methods findings and identify multilevel intervention strategies to prevent stimulant-involved overdoses. DISCUSSION: Completion of this study will yield a rich understanding of the social epidemiology of stimulant and opioid-involved overdoses in addition to community-derived intervention strategies that can be readily implemented and scaled to prevent such overdoses in two states disproportionately impacted by the opioid and overdose crises: Massachusetts and Rhode Island.


Assuntos
Overdose de Drogas , Humanos , Overdose de Drogas/prevenção & controle , Overdose de Drogas/epidemiologia , Rhode Island/epidemiologia , Estimulantes do Sistema Nervoso Central/análise , Massachusetts/epidemiologia , Fatores de Risco , Fentanila/intoxicação , Fentanila/análise
2.
J Anal Toxicol ; 48(7): 514-518, 2024 Aug 21.
Artigo em Inglês | MEDLINE | ID: mdl-38937871

RESUMO

Brain can be a useful specimen for toxicology testing as it is a protected and isolated organ with lower metabolic activity than other tissues, but there is currently no published data supporting the stability of stimulant drugs in prepared brain homogenates. Brain homogenates were evaluated to determine the stability of the following stimulant drugs: amphetamine, benzoylecgonine, bupropion, cocaethylene, cocaine, ephedrine, methylenedioxyamphetamine, methylenedioxymethamphetamine, methamphetamine, and phentermine. Four different homogenates were prepared at a 1:4 dilution with deionized water and fortified at 500 ng/mL of: cocaine without sodium fluoride, cocaine with 1% sodium fluoride, stimulant drugs other than cocaine without sodium fluoride, and stimulant drugs other than cocaine with 1% sodium fluoride. The fortified homogenates were aliquoted into 13 × 100-mm screw cap tubes and stored at room temperature (∼20°C), refrigerated (2-8°C), or frozen (<-5°C) and analyzed in triplicate on Days 0, 1, 3, 7, 14, 30, 60, and 90. Analytes were considered stable as long as the difference in analyte/internal standard response ratio from Day 0 was less than 20% and the peaks met qualitative acceptance criteria. All analytes were stable for up to 90 days when stored frozen with or without sodium fluoride and had variable stability at all other evaluated conditions.


Assuntos
Encéfalo , Estimulantes do Sistema Nervoso Central , Cocaína , Estabilidade de Medicamentos , Estimulantes do Sistema Nervoso Central/análise , Cocaína/análogos & derivados , Encéfalo/metabolismo , Detecção do Abuso de Substâncias/métodos , Metanfetamina/análogos & derivados , Metanfetamina/análise , Efedrina/análise , Efedrina/análogos & derivados , Fluoreto de Sódio , Bupropiona/análise , Anfetamina/análise , Animais
3.
J Anal Toxicol ; 48(5): 254-262, 2024 Jun 11.
Artigo em Inglês | MEDLINE | ID: mdl-38706158

RESUMO

Illegal amphetamine is usually composed of a racemic mixture of the two enantiomers (S)- and (R)-amphetamine. However, when amphetamine is used in medical treatment, the more potent (S)-amphetamine enantiomer is used. Enantiomer-specific analysis of (S)- and (R)-amphetamine is therefore used to separate legal medical use from illegal recreational use. The aim of the present study was to describe our experience with enantiomer-specific analysis of amphetamine in urine and oral fluid, as well as blood, and examine whether the distribution of the two enantiomers seems to be the same in different matrices. We investigated 1,722 urine samples and 1,977 oral fluid samples from prison inmates, and 652 blood samples from suspected drugged drivers, where prescription of amphetamine was reported. Analyses were performed using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS-MS). The enantiomer separation was achieved by using a chiral column, and results from the method validation are reported. Samples containing <60% (S)-amphetamine were interpreted as representing illegal use of amphetamine. The distribution of the two enantiomers was compared between different matrices. In urine and oral fluid, the mean amount of (S)-amphetamine was 45.2 and 43.7%, respectively, while in blood, the mean amount of (S)-amphetamine was 45.8%. There was no statistically significant difference in the amount of (S)-amphetamine between urine and oral fluid samples and between urine and blood samples, but the difference was significant in blood compared to oral fluid samples (P < 0.001). Comparison of urine and oral fluid between similar populations indicated that enantiomers of amphetamine can be interpreted in the same way, although marginally higher amounts of (R)-amphetamine may occur in oral fluid. Oral fluid, having several advantages, especially during collection, could be a preferred matrix in testing for illegal amphetamine intake in users of medical amphetamine.


Assuntos
Anfetamina , Saliva , Detecção do Abuso de Substâncias , Espectrometria de Massas em Tandem , Humanos , Anfetamina/urina , Anfetamina/sangue , Anfetamina/análise , Saliva/química , Estereoisomerismo , Detecção do Abuso de Substâncias/métodos , Cromatografia Líquida de Alta Pressão , Estimulantes do Sistema Nervoso Central/urina , Estimulantes do Sistema Nervoso Central/sangue , Estimulantes do Sistema Nervoso Central/análise
4.
Addiction ; 119(6): 1013-1020, 2024 06.
Artigo em Inglês | MEDLINE | ID: mdl-38509858

RESUMO

BACKGROUND AND AIMS: The use and manufacture of methamphetamine has increased in Afghanistan in recent years. Recent research and reports have pointed to the ephedra plant, which grows wildly, as a key source of ephedrine used in the manufacture of methamphetamine. This paper aimed to estimate the relative efficiencies and scale of inputs required to manufacture methamphetamine in Afghanistan. METHODS: Monte Carlo simulations model of the amount of ephedra or cold medications needed to render a pure kilogram of methamphetamine in Afghanistan, accounting for uncertainty in ranges of key parameters informed from the literature and elsewhere. Final estimates were extrapolated to recent seizure totals. RESULTS: For dried ephedra, the median estimate is 196.8 kg (25th-75th percentiles 119.3-346.6 kg) needed to produce 1 kg of methamphetamine compared with 27.9 kg (25th-75th percentiles 21.9-36.8 kg) for cold medications. Nearly 2.7 t of methamphetamine were seized in Afghanistan in 2021. Assuming a purity range of 50%-90%, some 266-478 t of dried ephedra or 38-68 t of cold medication would need to have been processed. CONCLUSION: Simulated estimates show that considerable amounts of either ephedra or cold medication are needed to produce 1 kg of methamphetamine in Afghanistan. This raises questions about the plausibility of ephedra as the dominant source of Afghanistan's methamphetamine.


Assuntos
Metanfetamina , Método de Monte Carlo , Metanfetamina/análise , Afeganistão , Humanos , Ephedra , Estimulantes do Sistema Nervoso Central/análise , Efedrina/análise , Drogas Ilícitas/análise
5.
Forensic Sci Int ; 356: 111966, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38367459

RESUMO

Amphetamine-type stimulants are the third most widely consumed category of illicit drugs worldwide. Faced with the growing problem of amphetamine-type stimulants, numerous qualitative and quantitative techniques have been developed to detect amphetamine (AMP), methamphetamine (MET), MDMA, MDEA or MDA in biological matrices, including hair. Hair analysis is widely used in forensic medicine, but one of its main drawbacks remains external contamination. In this study, we investigated the possibility of hair contamination through external exposure to blood containing AMP, MET MDMA, MDEA or MDA at 2 ng/mL; 20 ng/mL; 200 ng/mL or 2000 ng/mL after 6 h, 1, 3, 7 or 14 days of contact protected from light at room temperature (RT or 20 °C) or at 4 °C. Dried extracts of hair samples were analyzed by UPLC-MS/MS after extensive washings in several baths of water, methanol and acetone before grounding. At the end of our study, contamination of hair was observed from 6 h of contact with all tested amphetamine-type stimulants. The concentrations found in hair ranged from 3 ± 1 to 1464 ± 10 pg/mg, 5 ± 1 to 5070 ± 160 pg/mg, 3 ± 1 to 1269 ± 60 pg/mg, 4 ± 1 to 1860 ± 113 pg/mg and from 8 ± 1 to 1041 ± 44 pg/mg for AMP, MET, MDMA, MDEA and MDA, respectively. Possibly due to its low polar surface area, MET was the most prone to contaminate. As anticipated, hair contamination was mainly dependent on the concentration of all molecules in the contaminating blood, reaching the SOHT cut-off of 200 pg/mg when amphetamine-type stimulants are at toxic or lethal concentrations in the blood. These observations call for caution in interpreting exposure to these substances in such forensic situations.


Assuntos
3,4-Metilenodioxianfetamina/análogos & derivados , Estimulantes do Sistema Nervoso Central , Metanfetamina , N-Metil-3,4-Metilenodioxianfetamina , Anfetaminas/análise , Cromatografia Líquida , Espectrometria de Massas em Tandem , Detecção do Abuso de Substâncias/métodos , Estimulantes do Sistema Nervoso Central/análise , Cabelo/química
6.
J Forensic Sci ; 69(3): 1011-1020, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38351585

RESUMO

Recreational methamphetamine production and heavy use can result in dwelling contamination that is difficult to detect. First responders and public health officials may use commercially available trace methamphetamine detection (presumptive) test kits to understand apparent and hidden dangers in impacted dwellings. Here, we assessed the limit of detection (LOD) of several commercially available presumptive test kits using simulated contaminated hard surfaces. Pyrex petri dishes were spiked with aliquots of methanolic methamphetamine solutions to reach desired simulated contamination levels. Commercially available presumptive tests were conducted according to manufacturer instructions and using included sample preparation materials, when available. Additionally, a laboratory-based liquid chromatography-triple quadrupole mass spectrometer (LC-MS/MS) trace methamphetamine quantification method was developed and validated using the EZSTATSG2 tool. For the LC-MS/MS method, samples were collected using 2-ply alcohol prep pads and methamphetamine was extracted using a 1:1 (v:v) methanol: water solution. Most presumptive tests considered were able to detect trace levels of methamphetamine extracted from hard surfaces, with LOD ranging from 0.10-15.00 µg/sample. Comparatively, the laboratory-based LC-MS/MS LOD was 0.05 µg/sample and limit of quantitation was 0.10 µg/sample. The LC-MS/MS method may be useful when the presence of dust or other contaminants interferes with presumptive test interpretation or reliability. Costs of presumptive tests varied from several dollars to tens of dollars, which is included alongside LOD results to aid stakeholders in identifying which test(s) are the best fit for purpose. Therefore, first responders, public health officials, and other stakeholders have several options for assessing trace methamphetamine contamination.


Assuntos
Toxicologia Forense , Limite de Detecção , Metanfetamina , Metanfetamina/análise , Cromatografia Líquida , Humanos , Toxicologia Forense/métodos , Estimulantes do Sistema Nervoso Central/análise , Espectrometria de Massas em Tandem , Propriedades de Superfície , Espectrometria de Massas/métodos , Espectrometria de Massa com Cromatografia Líquida
7.
J Forensic Sci ; 69(3): 1021-1024, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38362738

RESUMO

The conventional methamphetamine (MA) detection method using the Simon reaction can be affected by false positives owing to compounds similar to aliphatic secondary amines. In this study, we examined the new Simon reaction to improve the qualitative accuracy of MA detection to discriminate substances that give false positives in a conventional Simon reaction. After the conventional Simon reaction for MA and false positives (N-isopropylbenzylamine (NIP-BA), N-methylbenzylamine (NMe-BA), L-proline (Pro), and L-hydroxyproline (HYP)), which are colored blue, di-tert-butyl dicarbonate (t-Boc) reagent was added, and color tone changes were observed. When t-Boc was added to the false positives (NIP-BA, NMe-BA, Pro, and HYP), the colors of MA, Pro, and HYP changed to purple; NIP-BA changed to blue; and NMe-BA changed to light pink after 3 min. These results suggested that MA can be differentiated from NIP-BA and NMe-BA. Furthermore, the solid-phase chromogenic method was examined, and it was confirmed that MA could be differentiated from Pro and HYP. The method developed in this study should increase the accuracy of MA appraisal at crime scenes and contribute to the reduction of misclassifications arising from false-positive substances.


Assuntos
Toxicologia Forense , Metanfetamina , Humanos , Reações Falso-Positivas , Toxicologia Forense/métodos , Estimulantes do Sistema Nervoso Central/análise , Cor
8.
Forensic Toxicol ; 42(2): 232-241, 2024 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-38240998

RESUMO

PURPOSE: Intravenous narcotic agents, such as etomidate and metomidate, has been widely spread and abused in the world, including in Korea and China; thus, it is important to establish validated and sensitive analytical method for these compounds. Human hair as a biological sample has various advantages, including a wide detection window of drugs, compared to other typical samples, such as urine and blood in investigation. The purpose of this communication is to develop a reliable and useful method for the simultaneous detection and quantification of etomidate and metomidate in human hair samples by ultraperformance liquid chromatography combined with triple quadrupole mass spectrometry (UPLC-MS/MS), and to apply it for authentic samples in abuse cases. METHODS: The hair samples were washed with a detergent solution, followed by with water and acetone. After drying, they were cut into approximately 2 mm sections and then ground to powder by a low-temperature grinder. The 20 mg of hair powder plus internal standard in 1 mL of methanol was vortexed and then centrifuged to obtain the supernatant layer, followed by subjecting to analysis. RESULTS: The coefficient of determination (r2) values of the calibration curves of etomidate and metomidate in the hair samples were both more than 0.99 in the range of 1-500 ng/mg and 1-500 pg/mg, respectively. The limits of detection and lower limits of quantification were 0.5 and 1 pg/mg, respectively, for the both target compounds. Other tested validation data were all satisfactory. Etomidate and metomidate could be detected in the all hair samples and cigarette oil, which were seized by the police. The concentrations of etomidate and metomidate obtained from 10 samples from suspects were 5.48-45.7 ng/mg and 3.60-377 pg/mg, respectively. The concentrations of etomidate and metomidate in the cigarette oil were 95.8 µg/mg and 2.8 µg/mg, respectively. CONCLUSIONS: In this study, a simple and reliable analytical method for etomidate and metomidate in the human hair has been established. To the best of our knowledge, this is the first report to establish a method for the simultaneous detection and quantification of etomidate and metomidate in the human hair, and to apply it to authentic samples seized in authentic cases.


Assuntos
Etomidato , Cabelo , Detecção do Abuso de Substâncias , Humanos , Etomidato/análogos & derivados , Etomidato/análise , Cabelo/química , Detecção do Abuso de Substâncias/métodos , Cromatografia Líquida/métodos , Toxicologia Forense/métodos , Estimulantes do Sistema Nervoso Central/análise , Espectrometria de Massas em Tandem/métodos , Limite de Detecção , Espectrometria de Massas/métodos , Cromatografia Líquida de Alta Pressão/métodos , Metilfenidato/análogos & derivados , Metilfenidato/análise , Masculino , Espectrometria de Massa com Cromatografia Líquida
9.
Forensic Sci Int ; 344: 111597, 2023 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-36801502

RESUMO

The actual illicit market for synthetic drugs is characterized by a wide variety of psychoactive substances of different chemical and pharmacological classes, such as amphetamine-type stimulants and new psychoactive substances. The knowledge about its chemical composition, as well as the nature and quantity of the active substances present, is important for emergency care in intoxication cases by these substances and to establish adequate chemical and toxicological analysis procedures in forensic laboratories. The aim of this work was to study the prevalence of amphetamine-type stimulants and new psychoactive substances in the states of Bahia and Sergipe, in the northeast region of Brazil, involving samples of drugs seized by the local police forces from 2014 to 2019. In a total of 121 seized and analyzed samples, in which ecstasy tablets predominated (n = 101), nineteen substances were identified using GC-MS and 1D NMR techniques, comprising classical synthetic drugs and new psychoactive substances (NPS). In order to determine the composition of ecstasy tablets, an analytical method based on GC-MS was applied after validation. Analyzes of 101 ecstasy tablets showed that MDMA was the main substance, being found in 57% of the samples, in amounts between 27.3 and 187.1 mg per tablet. In addition, mixtures of MDMA, MDA, synthetic cathinones and caffeine were observed in 34 samples. These results demonstrate that the variety of substances found and the composition of seized materials in northeast Brazil is similar to other studies carried out previously in other Brazilian regions.


Assuntos
Estimulantes do Sistema Nervoso Central , Drogas Ilícitas , N-Metil-3,4-Metilenodioxianfetamina , Medicamentos Sintéticos , N-Metil-3,4-Metilenodioxianfetamina/análise , Brasil , Cromatografia Gasosa-Espectrometria de Massas , Drogas Ilícitas/análise , Estimulantes do Sistema Nervoso Central/análise , Anfetamina/análise , Comprimidos , Psicotrópicos/análise
10.
J Anal Toxicol ; 46(9): 991-998, 2023 Jan 24.
Artigo em Inglês | MEDLINE | ID: mdl-34792146

RESUMO

Urine is initially collected from athletes to screen for the presence of illicit drugs. Sweat is an alternative sample matrix that provides advantages over urine including reduced opportunity for sample adulteration, longer detection-time window and non-invasive collection. Sweat is suitable for analysis of the parent drug and metabolites. In this study, a method was developed and validated to determine the presence of 13 amphetamine- and cocaine-related substances and their metabolites in sweat and urine using disposable pipette extraction (DPX) by gas chromatography coupled to mass spectrometry. The DPX extraction was performed using 0.1 M HCl and dichloromethane:isopropanol:ammonium hydroxide (78:20:2, v/v/v) followed by derivatization with N-methyl-N-(trimethylsilyl) trifluoroacetamide at 90°C for 20 min. DPX extraction efficiencies ranged between 65.0% and 96.0% in urine and 68.0% and 101.0% in sweat. Method accuracy was from 90.0% to 104.0% in urine and from 89.0% to 105.0% in sweat. Intra-assay precision in urine and in sweat were <15.6% and <17.8%, respectively, and inter-assay precision ranged from 4.70% to 15.3% in urine and from 4.05% to 15.4% in sweat. Calibration curves presented a correlation coefficient -0.99 for all analytes in both matrices. The validated method was applied to urine and sweat samples collected from 40 professional athletes who knowingly took one or more of the target illicit drugs. Thirteen of 40 athletes were positive for at least one drug. All the drugs detected in the urine were also detected in sweat samples indicating that sweat is a viable matrix for screening or confirmatory drug testing.


Assuntos
Estimulantes do Sistema Nervoso Central , Cocaína , Dopagem Esportivo , Drogas Ilícitas , Humanos , Suor/química , Cromatografia Gasosa-Espectrometria de Massas/métodos , Espectrometria de Massas , Estimulantes do Sistema Nervoso Central/análise , Cocaína/análise , Drogas Ilícitas/análise
11.
Artigo em Inglês | MEDLINE | ID: mdl-35716546

RESUMO

The aim of this study was to develop a quantitative method for the analysis of methylphenidate, the analog ethylphenidate and their metabolite ritalinic acid in oral fluid, using micro-QuEChERS extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Oral fluid samples were collected with Quantisal™ device, extracted by micro-QuEChERS technique and analyzed by LC-MS/MS. The developed method met the validation criteria of Academy Standards Board (ASB) Standard Practices for Method Validation in Forensic Toxicology (Standard 036, 2019) with limits of detection and quantification of 0.5 ng/mL and calibration curve from 0.5 to 50 ng/mL. Within-run imprecision was greater than 18.7% while between-run imprecision was greater than 17.0 % for all analytes. Bias did not vary more than 7.7 %. No evidence of carryover was found. Stability studies presented satisfactory results for 24 h on autosampler (10 °C), after 3 cycles of freeze/thaw, 7 days on freezer (-20 °C) and until 7 days on refrigerator (4 °C) for methylphenidate. The validated method was further successfully applied to the analysis of 5 authentic oral fluid samples collected from volunteers at parties and music festivals from different cities in Brazil. Four samples had positive results for methylphenidate and ritalinic acid, and only one sample was positive for methylphenidate. Ethylphenidate was not detected in the samples. The method showed acceptable analytical performance and is environmentally friendly, requiring reduced use of solvents and reagents, with potential to be applied to clinical and forensic analyses.


Assuntos
Estimulantes do Sistema Nervoso Central , Metilfenidato , Estimulantes do Sistema Nervoso Central/análise , Cromatografia Líquida/métodos , Humanos , Metilfenidato/análogos & derivados , Espectrometria de Massas em Tandem/métodos
12.
Med. leg. Costa Rica ; 39(1)mar. 2022.
Artigo em Espanhol | LILACS, SaludCR | ID: biblio-1386305

RESUMO

Resumen El análisis por toxicomanía representa un proceso común solicitado por la Autoridad Judicial para determinar si un usuario presenta hallazgos compatibles con el uso de una droga a nivel clínico, componentes histológicos, patológicos y toxicológicos que puedan generar su uso. Es necesario destacar las limitaciones del ambiente clínico donde se pueden generar múltiples hallazgos, y de la toxicología forense donde a pesar de la especificidad a la que se asocia; también se encuentra limitada por la capacidad de sus equipos tecnológicos. La resonancia magnética nuclear cuantitativa de hidrógeno representa grandes ventajas al demostrar la presencia de una droga ilegal, así como la posibilidad de disminuir costos y tiempo laboral. El uso del MDMA como tratamiento con una reciente aprobación para un estudio de fase III por la FDA, también requiere que se valore el motivo de su uso, por lo que para realizar un análisis médico legal se contemplaron diversos elementos de juicio a fin de satisfacer la evaluación sobre la toxicomanía por MDMA en un usuario que presentó un tejido granular blanco tipo polvo en la sección distal del tabique nasal y negó el consumo de metanfetaminas.


Abstract The analysis for drug addiction represents a common process requested by the Judicial Authority to determine if a user presents findings compatible with the use of a drug at a clinical level, histological, pathological and toxicological components that may generate its use. It is necessary to highlight the limitations of the clinical environment where multiple findings can be generated, and of forensic toxicology where despite the specificity to which it is associated; it is also limited by the capacity of its technological equipment. Quantitative hydrogen nuclear magnetic resonance represents great advantages when demonstrating the presence of an illegal drug, as well as the possibility of reducing costs and labor time. The use of MDMA as a treatment with a recent approval for a phase III study by the FDA, also requires that the reason for its use be assessed, therefore, in order to carry out a legal medical analysis, various elements of judgment were considered in order to satisfy evaluation of MDMA drug addiction in a user who presented with white powder-like granular tissue in the distal section of the nasal septum and denied the use of methamphetamine.


Assuntos
Humanos , N-Metil-3,4-Metilenodioxianfetamina , Transtornos Relacionados ao Uso de Substâncias/diagnóstico , Estimulantes do Sistema Nervoso Central/análise , Costa Rica
13.
Drug Test Anal ; 14(1): 110-121, 2022 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-34435749

RESUMO

Hair samples are frequently analyzed in order to characterize consumption patterns of drugs. However, the interpretation of new psychoactive substance (NPS) findings in hair remains difficult because of lacking data for comparison. In this study, selected postmortem hair samples (n = 1203) from 2008 to 2020 were reanalyzed for synthetic cathinones, piperazines, phenethylamines, hallucinogens, benzodiazepines and opioids to evaluate prevalence data and concentration ranges. Hair samples were extracted using a two-step extraction procedure and analyzed using a validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. Overall NPSs were detected in 381 cases (31.6%). Many cases were tested positive for more than one NPS in the same time span. A variety of NPS with a large range of concentrations was observed. For better comparability and interpretation of positive cases in routine work, quantitation data for 13 NPS were calculated as percentiles. The most frequently detected NPS in this study were N-ethylamphetamine, α-pyrrolidinovalerophenone, mephedrone, benzedrone, metamfepramone, and 4-fluoroamphetamine. In conclusion, a high prevalence of these drugs was observed from postmortem hair samples. The results show a growing use of many different NPSs by mainly young drug-using adults. Consequently, NPS screening procedures should be included in forensic toxicology. Our quantitative data may support other toxicologists in their assessment of NPS hair concentrations.


Assuntos
Analgésicos Opioides/análise , Benzodiazepinas/análise , Estimulantes do Sistema Nervoso Central/análise , Cabelo/química , Alucinógenos/análise , Adolescente , Adulto , Cromatografia Líquida/métodos , Feminino , Toxicologia Forense/métodos , Humanos , Drogas Ilícitas/análise , Masculino , Pessoa de Meia-Idade , Prevalência , Estudos Retrospectivos , Detecção do Abuso de Substâncias/métodos , Espectrometria de Massas em Tandem/métodos , Adulto Jovem
14.
Drug Test Anal ; 14(1): 56-71, 2022 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-34355528

RESUMO

The rise in popularity of 'designer' precursor compounds for the synthesis of amphetamine-type stimulants poses a significant challenge to law enforcement agencies. One such precursor is α-phenylacetoacetonitrile (APAAN). APAAN emerged in Europe in 2010 and quickly became one of the most popular precursors for amphetamine synthesis in that region. Previous literature has identified four APAAN-specific impurities formed in the synthesis of amphetamine; however, there is currently no research on the use of APAAN in the synthesis of methamphetamine, which is more likely to be employed in a non-European market. In this study methamphetamine was synthesised via three common clandestine methods: the Leuckart method and two reductive amination methods. We report the identification of five new impurities and two previously identified impurities characteristic for the use of APAAN in the synthesis of methamphetamine. The newly identified impurities were characterised by MS and NMR and determined to be (E)-3-(methylamino)-2-phenylbut-2-enenitrile, 3-(methylamino)-2-phenylbutanenitrile, 3-methyl-2,4-diphenylpentanedinitrile, 2-phenylbutyronitrile and 3-hydroxy-2-phenylbutanenitrile.


Assuntos
Estimulantes do Sistema Nervoso Central , Drogas Ilícitas , Metanfetamina , Estimulantes do Sistema Nervoso Central/análise , Estimulantes do Sistema Nervoso Central/síntese química , Estimulantes do Sistema Nervoso Central/química , Contaminação de Medicamentos , Drogas Ilícitas/análise , Drogas Ilícitas/síntese química , Drogas Ilícitas/química , Espectroscopia de Ressonância Magnética , Espectrometria de Massas , Metanfetamina/análise , Metanfetamina/síntese química , Metanfetamina/química
16.
Anal Bioanal Chem ; 413(16): 4237-4246, 2021 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-33948704

RESUMO

Methamphetamine (MA) is a highly addictive and illegal psychostimulant drug and is currently one of the most commonly abused illicit drugs in the world. The on-site rapid detection of trace amounts of MA and screening illicit drugs in clandestine laboratories is important for drug enforcement agencies and the forensic community in general. However, detecting methamphetamine in the presence of nicotine and cigarette smoke by ion mobility spectrometry faces difficulty due to the overlapped spectral peaks of methamphetamine and nicotine. In this work, a new method was developed to detect MA using pyridine as a dopant in the presence of nicotine by a homemade ion mobility spectrometry. The reduced mobilities of MA and nicotine were measured under the temperatures of the drift tube from 40 to 120 °C and doping with pyridine. The result shows that the temperature of 100 °C is beneficial to resolve the two substances. The concentration of doped pyridine is optimized to be 18 ppm. In this doped experiment, the reaction rate of nicotine is higher than that of MA by measuring the instrumental responses of MA and nicotine. No matter how high the nicotine content is, the interference of nicotine can be eliminated in the detection of MA doped with pyridine. This method is also successfully applied for the determination of MA and nicotine simultaneously in real saliva samples. The limit of detection of MA was measured to be about 0.5 ng/µL. The promising results in this work provide an effective method for on-site detection of MA.


Assuntos
Estimulantes do Sistema Nervoso Central/análise , Metanfetamina/análise , Nicotina/análise , Saliva/química , Humanos , Drogas Ilícitas/análise , Espectrometria de Mobilidade Iônica/métodos , Limite de Detecção , Piridinas/química , Detecção do Abuso de Substâncias/métodos
17.
Clin Toxicol (Phila) ; 59(11): 975-981, 2021 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-33755516

RESUMO

BACKGROUND: Weight loss and sports supplements containing deterenol have been associated with serious adverse events including cardiac arrest. OBJECTIVE: To determine the presence and quantity of experimental stimulants in dietary supplements labeled as containing deterenol sold in the United States. METHODS: Dietary supplements available for sale in the US and labeled as containing deterenol or one of its synonyms (e.g., isopropylnorsynephrine and isopropyloctopamine) were purchased online. For each brand, one container or subsample was analyzed by NSF International (Ann Arbor, MI) and one container or subsample by the Netherland's National Institute for Public Health and the Environment (RIVM, Bilthoven, The Netherlands). When differences existed between the two containers or subsamples of the same brand, both products were reanalyzed by Sciensano (Brussels, Belgium). NSF International carried out qualitative and quantitative analyses using ultra-high-performance liquid chromatography (UHPLC) quadrupole-Orbitrap mass spectrometry. RIVM performed qualitative and quantitative analysis using UHPLC quadrupole time-of-flight mass spectrometry. Sciensano carried out qualitative analysis using UHPLC quadrupole-Orbitrap mass spectrometry. RESULTS: Seventeen brands of supplements were analyzed. Many brands included more than one prohibited stimulant in the same product: 4 brands (24%, 4/17) included 2 stimulants, 2 (12%, 2/17) combined 3 stimulants, and 2 (12%, 2/17) combined 4 stimulants. The range of quantities per recommended serving size of the 9 stimulants detected were 2.7 mg to 17 mg of deterenol; 1.3 mg to 20 mg of phenpromethamine (Vonedrine); 5.7 mg to 92 mg of beta-methylphenylethylamine (BMPEA); 18 mg to 73 mg of octodrine; 18 mg to 55 mg of oxilofrine; 48 mg of higenamine; 17 mg of 1,3-dimethylamylamine (1,3-DMAA); 1.8 mg to 6.6 mg of 1,3-dimethylbutylamine (1,3-DMBA); and 5.3 mg of 1,4-dimethylamylamine (1,4-DMAA). CONCLUSION: Weight loss and sports supplements listing deterenol as an ingredient contained 9 prohibited stimulants and 8 different mixtures of stimulants, with as many as 4 experimental stimulants per product. These cocktails of stimulants have never been tested in humans and their safety is unknown.


Assuntos
Agonistas Adrenérgicos/análise , Fármacos Antiobesidade/análise , Estimulantes do Sistema Nervoso Central/análise , Suplementos Nutricionais/análise , Agonistas Adrenérgicos/efeitos adversos , Alcaloides/análise , Aminas/análise , Anfetaminas/análise , Fármacos Antiobesidade/efeitos adversos , Estimulantes do Sistema Nervoso Central/efeitos adversos , Qualidade de Produtos para o Consumidor , Suplementos Nutricionais/efeitos adversos , Efedrina/análogos & derivados , Efedrina/análise , Heptanos/análise , Humanos , Octopamina/análogos & derivados , Octopamina/análise , Medição de Risco , Tetra-Hidroisoquinolinas/análise , Estados Unidos
18.
Forensic Sci Int ; 321: 110746, 2021 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-33676238

RESUMO

A more than 500% increase in the number of deaths involving methamphetamine occurred between 2016 and 2018 in Jeddah, Saudi Arabia. As such, this report employed a validated liquid chromatography tandem mass spectrometry method to quantify methamphetamine and its metabolites in bodily fluids from 47 postmortem cases in which methamphetamine was involved. The mean age of the deceased was 33 years old (median: 30, range: 16-63), and 94% were male. Methamphetamine was co-ingested with another drug in 32 of the cases (68%); however, the deaths were only due to the combined toxicity of methamphetamine and another drug in 15 of the cases (32%). Of note, 13 of these deaths (28% of all deaths) involved heroin. When methamphetamine was the sole cause of death (32% of the studied cases), the median concentrations of methamphetamine and amphetamine were 527 and 128 ng/mL. When methamphetamine was combined toxicity with another drug, the median concentrations of methamphetamine and amphetamine decreased to 161 and 53 ng/mL. When deaths were unrelated to methamphetamine, the median concentrations of methamphetamine and amphetamine were 130 and 44 ng/mL, respectively. The highest median methamphetamine concentration was found in urine (5281 ng/mL), followed by stomach contents (878 ng/mL), bile (762 ng/mL), vitreous humor (3 ng/mL), and blood (208 ng/mL). Almost 40% of the studied cases involved violence, 61% were accidental, 21% were suicides, 17% were homicides, and 2% were natural deaths. Methamphetamine is highly addictive. Increases in deaths have been seen in various countries. More awareness, education and treatment programs are required to reduce the likelihood of addiction, crimes, suicide, and other fatalities resulting from methamphetamine abuse.


Assuntos
Transtornos Relacionados ao Uso de Anfetaminas/mortalidade , Estimulantes do Sistema Nervoso Central/intoxicação , Metanfetamina/intoxicação , Acidentes/estatística & dados numéricos , Adolescente , Adulto , Distribuição por Idade , Bile/química , Estimulantes do Sistema Nervoso Central/análise , Feminino , Conteúdo Gastrointestinal/química , Homicídio/estatística & dados numéricos , Humanos , Masculino , Metanfetamina/análise , Pessoa de Meia-Idade , Arábia Saudita/epidemiologia , Distribuição por Sexo , Detecção do Abuso de Substâncias , Suicídio Consumado/estatística & dados numéricos , Corpo Vítreo/química , Adulto Jovem
19.
ACS Appl Mater Interfaces ; 13(2): 3024-3032, 2021 Jan 20.
Artigo em Inglês | MEDLINE | ID: mdl-33404230

RESUMO

A wearable surface-enhanced Raman scattering (SERS) sensor has been developed as a patch type to utilize as a molecular sweat sensor. Here, the SERS patch sensor is designed to comprise a sweat-absorbing layer, which is an interface to the human skin, an SERS active layer, and a dermal protecting layer that prevents damage and contaminations. A silk fibroin protein film (SFF) is a basement layer that absorbs aqueous solutions and filtrates molecules larger than the nanopores created in the ß-sheet matrix of the SFF. On the SFF layer, a plasmonic silver nanowire (AgNW) layer is formed to enhance the Raman signal of the molecules that penetrated through the SERS patch in a label-free method. A transparent dermal protecting layer (DP) allows laser penetration to the AgNW layer enabling Raman measurement through the SERS patch without its detachment from the surface. The molecular detection capability and time-dependent absorption properties of the SERS patch are investigated, and then, the feasibility of its use as a wearable drug detection sweat sensor is demonstrated using 2-fluoro-methamphetamine (2-FMA) on the human cadaver skin. It is believed that the developed SERS patch can be utilized as various flexible and wearable biosensors for healthcare monitoring.


Assuntos
Técnicas Biossensoriais/instrumentação , Análise Espectral Raman/instrumentação , Suor/química , Dispositivos Eletrônicos Vestíveis , Animais , Bombyx/química , Estimulantes do Sistema Nervoso Central/análise , Monitoramento de Medicamentos/instrumentação , Fibroínas/química , Humanos , Metanfetamina/análogos & derivados , Metanfetamina/análise , Nanofios/química , Prata/química , Propriedades de Superfície
20.
Anal Bioanal Chem ; 413(8): 2147-2161, 2021 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-33517480

RESUMO

Resolution of cathinone enantiomers in equine anti-doping analysis is becoming more important to distinguish the inadvertent ingestion of plant-based products from those of deliberate administration of designer synthetic analogs. With this in mind, a rapid and sensitive method was developed and validated for the detection, resolution and quantitative determination of cathinone enantiomers in horse blood plasma and urine. The analytes were recovered from the blood plasma and urine matrices by using a liquid-liquid extraction after adjusting the pH to 9. The recovered analytes were derivatized with Nα-(2,4-dinitro-5-fluorophenyl)-L-valinamide, a chiral derivatizing agent analogous to Marfey's reagent. The resulting diastereoisomers were baseline resolved under a reversed-phase liquid chromatographic condition. Derivatization of the analytes not only allowed the separation of the enantiomers using cost-effective traditional liquid chromatography conditions and reversed-phase columns but also increased the sensitivity, at least to an order of magnitude, when tandem mass spectrometry is used for the detection. A limit of detection of 0.05 ng/mL was achieved for cathinone enantiomers for both matrices. Acceptable intraday and interday precision and accuracy along with satisfactory dilution accuracy and precision were observed during the method validation. The method suitability was tested using the post administration urine samples collected after single doses of cathinone and ephedrine as single-enantiomeric form and methcathinone as racemic form. Finally, a proof of concept of the isomeric ratio in urine samples to distinguish the presence of cathinone as a result of accidental ingestion of plant-based product from that of an illicit use of a designer product is demonstrated. To the best of our knowledge, this is the first such work where cathinone enantiomers were resolved and quantified in horse blood plasma and urine at sub nanogram levels.


Assuntos
Alcaloides/sangue , Alcaloides/urina , Estimulantes do Sistema Nervoso Central/sangue , Estimulantes do Sistema Nervoso Central/urina , Cavalos/sangue , Cavalos/urina , Alcaloides/análise , Animais , Estimulantes do Sistema Nervoso Central/análise , Cromatografia Líquida de Alta Pressão/métodos , Dopagem Esportivo , Limite de Detecção , Estereoisomerismo , Detecção do Abuso de Substâncias/métodos , Espectrometria de Massas em Tandem/métodos
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