Letícia Birk

Ecstasy-type drugs are the most frequently seized synthetic drugs in Brazil, usually containing a mixture of MDMA and its analog MDA. In recent years, an increasing number of samples have been found to contain only MDA, possibly reflecting shifts in the synthetic routes of ecstasy-type substances during the COVID-19 pandemic. However, the exclusive use of MDA remains poorly characterized, and its toxicological profile is still not fully understood. Data from chemical analyses of drug seizures in Rio Grande do Sul, Southern Brazil, were reviewed. In addition, blood and urine samples collected from clinical and forensic cases involving ecstasy use were analyzed by LC-MS/MS. MDA was detected in 31.1% of seized drug samples, surpassing MDMA, which accounted for 25.6%. A marked rise in MDA detections was observed after 2020, peaking at 52.6% of seizures in 2023. In addition, sixteen clinical and four postmortem cases involving MDMA and/or MDA were documented, with MDA predominating from 2021 onwards. The study identified a higher prevalence of MDA compared to MDMA, indicating a shift in ecstasy use patterns in Brazil. This finding underscores the need for robust analytical approaches and sustained toxicological monitoring to support drug surveillance and public health policies.

Drug use affects a significant portion of the Brazilian population, which increases the likelihood of children being exposed to illicit drug environments, making them a particularly vulnerable group. This study describes the profile of illicit drug exposure in children up to 12 years in Rio Grande do Sul state, Brazil, based on emergency cases. Data were collected from suspected intoxication cases attended between 2018 and 2023 in children ≤12 years old. Urine samples were analyzed for cocaine and its metabolites, THC-COOH, and amphetamine-type stimulants using LC-MS/MS. Information about the cases was also collected. Of 286 suspected cases, 32.9% detected at least one illicit drug. Cocaine and its metabolites were the most common (24.8%), followed by THC-COOH (9.4%) and MDA/MDMA (2.1%). Among detected drug cases, 56.4% were male. The mean age was 3.4 ± 3.5 years, with the highest incidence in 1 to 4-year-olds (47.9%). Exposure circumstances included accidental (37.2%), mistreatment/violence (8.5%), and abuse (2.1%). Most exposures occurred at home (58.5%). A notable prevalence of illicit drugs, mainly cocaine, was found. These data show a worrying scenario of drug exposure, primarily involving children aged 1 to 4 years. Above all, it also demonstrates a high frequency of exposure to illicit drugs in their own homes. The findings provide a solid basis for toxicovigilance activities and the development of public health policies aimed at protecting the vulnerable pediatric population.

The laboratory analysis of new psychoactive substances and related drugs is crucial for accurate clinical and forensic diagnosis of poisonings. Given this, a new LC‐MS/MS method for analyzing hallucinogens, synthetic cathinones, and synthetic cannabinoids in urine was developed. Urine samples were extracted using a liquid–liquid extraction protocol optimized via a multivariate experimental design. An aliquot of 400 μL of urine was enzymatically hydrolyzed with β‐glucuronidase and extracted with 700 μL of ethyl acetate. The resulting extracts were analyzed using LC‐MS/MS, with a total chromatographic run time of 8 min. The method was validated according to the ANSI/ASB Standard 036 guideline and was applied to 24 samples from suspected poisoning cases. The lower limits of quantification ranged from 0.1 to 1 ng/mL. Within‐run and between‐run precision (CV) were < 16%, and bias ranged from −12.8% to 19.8%. Nine of the 20 analytes investigated showed significant ionization suppression or enhancement (> 25%). Only two analytes (2C‐E and 2‐oxo‐3‐OH‐LSD) had a recovery rate lower than 70%. Among the 24 analyzed urine samples, one tested positive for 25B‐NBOH, one for LSD, and two for 2‐oxo‐3‐OH‐LSD. The developed method enables the simultaneous quantification of 20 illicit drugs, serving as an efficient diagnostic tool for clinical and forensic laboratories.

The detection of new psychoactive substances in postmortem blood is of primary importance for the investigation of related deaths. A method using cork as a biosorbent in a solid-phase microextraction with LC-MS/MS analysis was developed and validated for the determination of synthetic cathinones and related substances in blood. The sample preparation method employed 200 µL of sample and 30 mg of cork powder, and the complete procedure was optimized using multivariate strategies. LC-MS/MS analysis was performed in gradient mode, with a total run time of 7.5 min for the determination of cathinone, ethylone, fentanyl, MDA, MDMA, mephedrone, N-ethylpentylone, and pentylone. Comprehensive validation was performed through the ASB/ANSI Standard 036. Lower limit of quantification (LLOQ) values ranged between 0.5 and 1 ng/mL, with linear ranges between LLOQ and 85 ng/mL. Accuracy and precision results were satisfactory, and significant ion suppression was found (2.9–63.4%). Applicability of the method was evaluated by the analysis of three postmortem blood samples from forensic casework, suspected to have the presence of synthetic cathinones. All samples were positive for MDMA and MDA, with concentrations between 79.2–198.1 ng/mL and 23.1–26.6 ng/mL, respectively. The greenness of the method was also evaluated by AGREEprep, with an overall score of 0.53. This study is the first to apply a cork-based extraction to blood analysis. The method has proven to be reliable and a valuable greener alternative for the determination of synthetic cathinones and related substances in postmortem blood. Graphical Abstract

Purpose Toxicological analyses of postmortem blood samples are essential to elucidate forensic cases involving toxic agents, such as illicit drugs. A simple method for determining stimulant substances in postmortem blood samples through protein precipitation and liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed and applied in nearly 1000 samples from Brazilian forensic cases. Methods For sample preparation, 100 µL of postmortem blood was precipitated using acetonitrile. The supernatant was analyzed via LC–MS/MS system for sixteen substances, including amphetamine, benzoylecgonine, cocaethylene, cocaine, diethylpropion, dimethyltryptamine, ecgonine methyl ester (EME), ephedrine, fenproporex, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxyethylamphetamine, 3,4-methylenedioxymethamphetamine, methamphetamine, methylphenidate, phenylephrine, and sibutramine. The method was validated following the parameters established by the ANSI/ASB Standard 036 Guideline. After validation, a total of 971 postmortem blood samples were analyzed. Results The lower limits of quantification varied from 5 to 20 ng/mL, with all substances demonstrating linearity up to 1000 ng/mL. The method exhibited maximum precision values of 19.3%, while the bias ranged from − 15.4 to + 4.3%. A significant matrix effect was observed only for EME and phenylephrine. Approximately 20.1% of the analyzed samples tested positive for at least one substance, and 12 out of the 16 target analytes were detected. The most prevalent substances identified were benzoylecgonine (17.8%), ecgonine methyl ester (13.9%), and cocaine (13.0%). Conclusions A rapid and straightforward LC–MS/MS method for the quantitative analysis of drugs in postmortem blood was validated and successfully applied to nearly 1000 postmortem blood samples.

Objective: This study investigated blood and salivary parameters in male resistance-training practitioners (RTP) using oxandrolone (OG) and compared with references values and control group (CG), in triplicate. Methods: Blood, saliva, and urine were collected from 22 individuals (OG, n = 11 / CG, n = 11) and analyzed: before oxandrolone (OX) consumption (T1), at cessation of OX use (T2), and three months after cessation of OX use (T3). Complete blood count, lipid profile, metabolites, and enzymes were analyzed from blood samples. Salivary flow, pH, triglycerides, urea, aspartate animotransferase, alanine aminotransferase, phosphorus, and calcium were analyzed from saliva. Urinalysis was used for toxicological screening. Results: A reduced hdl cholesterol level was observed in the og group (24 mg/dL) compared with the reference value (>40 mg/dL) at T2. HDL levels return to normal after cessation AT T3 (49 mg/dL, >40 mg/dL). A higher triglyceride level (177 mg/dL) was verified in OG group compared with the reference value (<175 mg/dL) at T3. Conclusions: The results of this study suggest that oxandrolone use is associated with changes in lipid profiles, including lower HDL levels and higher triglyceride levels, which are characteristic of dyslipidemia. however, while these findings indicate an association, they do not establish definitive causality. further research, including well-controlled longitudinal studies, is needed to confirm the causal relationship between oxandrolone use and dyslipidemia.

Cocaine and antidepressants rank high globally in substance consumption, emphasizing their impact on public health. The determination of these compounds and related substances in biological samples is crucial for forensic toxicology. This study focused on developing an innovative analytical method for the determination of cocaine, antidepressants, and their related metabolites in postmortem blood samples, using unmodified commercial Fe₃O₄ nanoparticles as a sorbent for dispersive magnetic solid-phase extraction (m-d-SPE), coupled with liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) analysis. An aliquot of 100 µL of whole blood and 5 µL of the internal standard pool were added to 30 mg of nanoparticles. The nanoparticles were separated from the sample using a neodymium magnet inserted into a 3D-printed microtube rack. The liquid was then discarded, followed by desorption with 300 µL of 1/1/1 acetonitrile/methanol/ethyl acetate. The sample was vortexed and separated, and 1.5 µL of the organic supernatant was injected into the LC–MS/MS. The method was acceptably validated and successfully applied to 263 postmortem blood samples. All samples evaluated in this study were positive for at least one substance. The most frequent analyte was benzoylecgonine, followed by cocaine and cocaethylene. The most common antidepressants encountered in the analyzed samples were citalopram and fluoxetine, followed by fluoxetine’s metabolite norfluoxetine. This study describes the first report of this sorbent in postmortem blood analysis, demonstrating satisfactory results for linearity, precision, accuracy, and selectivity for all compounds. The method’s applicability was confirmed, establishing it as an efficient and sustainable alternative to traditional techniques for forensic casework.

Over the last decades, new psychoactive substances (NPSs) have established a new pattern of drug synthesis and distribution. These compounds brought with them several challenges, including their analytical determination by known methodologies, the uncertainty of their toxicological effects, and the possible approaches used for control. In Brazil, the control of NPS started with a nominal list of proscribed compounds. But the variety of substances was so large that other strategies were implemented. Generic legislation was created as several groups began to emerge, such as phenethylamines, synthetic cathinones, and synthetic cannabinoids. The legislation also began to include salts and isomers of all listed substances and precursor chemical ingredients or plants that may be used to produce them. Those substances are known for the unpredictability of their effects, causing a wide range of symptoms, including seizures, aggression, and acute psychosis. Users under effect represent a high risk for themselves and others. In this study, we present an overview of the timeline in which NPSs were detected in Brazilian territory and the legislative approaches. A complete literature search was performed using PubMed, Scopus, the World Wide Web and Brazilian governmental websites employing relevant keywords such as NPS, legislation, and Brazil. Even with the high volume of legislative measures, the race against NPS intoxication cases and apprehensions continues to be fierce. There are limitations in the process of detection, identification, and prohibition of the substances in the country that demand a multifactorial approach, stronger public health measures, scientific research, as well as harm reduction strategies. Nevertheless, the Brazilian scenario on NPS arrival reflects a worldwide problem faced by many countries. In conclusion, it is stated that the use of multiple legislative strategies such as prohibition lists and generic controls can provide for better regulation of the NPS problem. However, this issue needs to be addressed by multiple organizations, including police departments and the public health system, and that effort needs to be coordinated and standardized for all Brazilian Federal states.

In recent years, the environmental implications of advancements in various scientific fields, including analytical chemistry, have become a subject of increasing concern. As a result, the concept of “Green Analytical Chemistry” has been developed, comprising a set of practices designed to reduce the use of toxic chemicals. In the field of analytical, minimizing chemical usage presents a significant challenge, as several sample preparation methods inherently require the utilization of large quantities of solvents. However, this challenge can be addressed through the implementation of both single and combined strategies. One of these strategies is the miniaturization of methods applying the principles of classic liquid–liquid and solid phase extractions in a smaller scale of reagents and samples. In addition, the conventional reagents used in sample preparation can be replaced with green solvents and sorbents. The utilization of miniaturized techniques in forensic toxicology has been widely adopted. Despite this, there remain numerous unexplored applications due to the vast diversity of analytes and biological matrices available. Therefore, implementing green chemistry practices can provide numerous benefits, including enhanced worker safety, reduced waste, and cost savings.This article is categorized under: Toxicology > Analytical Toxicology > Drug Analysis Toxicology > Post‐Mortem