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- Analysis of Cannabinoids in Biological Specimens: An UpdatePublication . Antunes, Mónica; Barroso, Mário; Gallardo, EugeniaCannabinoids are still the most consumed drugs of abuse worldwide. Despite being considered less harmful to human health, particularly if compared with opiates or cocaine, cannabis consumption has important medico-legal and public health consequences. For this reason, the development and optimization of sensitive analytical methods that allow the determination of these compounds in different biological specimens is important, involving relevant efforts from laboratories. This paper will discuss cannabis consumption; toxicokinetics, the most detected compounds in biological samples; and characteristics of the latter. In addition, a comprehensive review of extraction methods and analytical tools available for cannabinoid detection in selected biological specimens will be reviewed. Important issues such as pitfalls and cut-off values will be considered.
- UHPLC-MS/MS methodology for analysis of new synthetic opioids and hallucinogens in whole bloodPublication . Pereira, Joana; Antunes, Mónica; Neng, N.R.; Mustra, Carla; Franco, João; Fonseca, SuzanaBackground & Aims: New Psychoactive Substances (NPS) are a real contemporaneous threat, due to their potency, dangerousness, and lack of control/monitoring. The NPS group that has grown the most is the synthetic opioids group, where fentanyl and its analogues stand out. However, the emerging concerning synthetic opioids are nitazenes. Due to their high potency, even minimal consumption doses can lead to severe health effects or even fatal overdoses, making them a public health issue. Notwithstanding, is it also important to remain vigilant towards more “traditional” psychoactive substances like hallucinogens once they have been associated with both intentional and unintentional poisonings/intoxications. This is particularly relevant now that they are also being used for clinical purposes. Therefore, it is essential to establish analytical methodologies for monitoring these compounds. As a result, the aim of this study was to develop, optimize and validate an easy to use, fast, simple, sensitive, robust, and routine flow method for the analysis of new synthetic opioids (fentanyls and nitazenes) and (classic) hallucinogens in whole blood. Methods: The present work describes a method that allows the screening, qualitative confirmation, and quantification of more than 10 psychoactive substances, including new synthetic opioids and hallucinogens. The sample preparation step consisted in 50 µL of whole blood protein precipitation with refrigerated acetonitrile containing formic acid and was optimized using a design of experiments (DoE) approach, namely Full Factorial Design, to achieve the best conditions for compounds extraction from matrix. Following centrifugation, the resulting supernatant extract can be directly injected into an ultra-high-performance liquid chromatograph coupled to a triple quadrupole linear ion trap mass spectrometer (Sciex UHPLC-QTRAP-MS® 6500+) and analyzed in a 5-minute run in Multiple Reaction Monitoring (MRM) mode with 2 transitions for each compound. The developed analytical methodology was fully validated according to the guiding principles of the ANSI/ASB Standard 036. To confirm its applicability in a real context, the proposed methodology was applied to the analysis of authentic forensic samples. Results & Discussion: In terms of validation, the methodology linearity was assessed between 1 and 20 ng/mL. The precision and accuracy were satisfactory, with values <15% and within ±15% (20% at the LOQ), respectively. The limits of detection were between 0.1 and 1 ng/mL, depending on the compound. Dilution ratios were also successfully evaluated. Selectivity was confirmed by analyzing spiked samples containing several therapeutic drugs and other drugs of abuse. Conclusion: The proposed methodology provides a valuable and powerful tool for toxicology laboratory, enabling the simultaneous identification, confirmation, and quantification of different families of psychoactive substances, including synthetic opioids and hallucinogens. Its speed, simplicity, effectiveness, and reliability make it particularly advantageous for routine analysis. These combined advantages make it a suitable alternative for routine implementation.
- Development and validation of a simple and fast method for routine analysis of new synthetic opioids and hallucinogens in whole blood using protein precipitation and UHPLC-MS/MSPublication . Pereira, Joana R.P.; Antunes, Mónica; Neng, N.R.; Mustra, Carla; Franco, João; Fonseca, SuzanaIn forensic toxicology, the rapid and reliable detection of emerging synthetic opioids and hallucinogens is crucial for case investigations and public health monitoring. This work describes the development, optimization and validation of a simple, fast and sensitive methodology for the simultaneous analysis of 6 new synthetic opioids (carfentanil, fentanyl, isotonitazene, metonitazene, norfentanyl, and sufentanil) and 2 hallucinogens (lysergide [LSD] and mescaline), together with the main LSD metabolite 2-oxo-3-hydroxy-lysergide [LSD-OH], in whole blood samples by liquid chromatography coupled to tandem mass spectrometry. Under optimized experimental conditions, linearity was verified between 0.1 and 20 ng/mL for all analytes except mescaline (2.5-500 ng/mL), with r2 > 0.99 for 1/x weighting, and no significant carryover or matrix effects were observed. Good precision (% RSD < 13 %) and trueness (% Bias within ± 20 %) values were achieved. The estimated limit of quantification (LOQ) was 0.1 ng/mL for all compounds except mescaline (2.5 ng/mL). Authentic forensic samples were also analyzed, and positive samples for fentanyl, norfentanyl, and sufentanil were identified. The proposed methodology allows the simultaneous analysis of compounds from different families of psychoactive substances, in both postmortem and in vivo samples, using only 50 µL of whole blood. The demonstrated speed, simplicity, and effectiveness make it particularly advantageous for routine implementation in forensic toxicology laboratories.
- Detection and quantification of selected cannabinoids in hair samples by liquid-liquid extraction and LC-MS/MSPublication . Antunes, Mónica; Simões, Susana; Fonseca, Suzana; Franco, João; Barroso, Mário; Gallardo, EugeniaCannabis remains the most used illicit drug worldwide, with rising use linked to medical and recreational decriminalization. This has driven the development of analytical techniques to detect cannabinoids in biological matrices. Hair offers key advantages due to its non-invasive collection, extended detection window, stability, and easy storage. This study presents the development and validation of a robust method for extracting natural cannabinoids from hair, following ANSI/ASB 2019, FDA, and Society of Hair Testing guidelines. Hair samples were washed with methanol and cut into small pieces. Approximately 20 mg of hair was incubated with 1 M NaOH and methanol (30 min, 50 °C). The mixture was acidified with acetic acid and underwent liquid-liquid extraction using hexane/ethyl acetate (90/10, v/v). The organic phase was evaporated and reconstituted in 1-pentanol/methanol (50/50, v/v). Analysis was conducted by LC-MS/MS using multiple reaction monitoring (MRM) and triple-stage mass spectrometry (MS³). The method was selective, specific, precise, and linear, with working ranges of 5-2000 pg/mg for THC, CBN, and CBD; 50-2000 pg/mg for THC-OH; and 0.2-20 pg/mg for THC-COOH. Ion suppression was observed but did not affect sensitivity, with LLOQs and LODs from 0.2 to 50 pg/mg. Over 25 hair samples from university students tested positive for cannabis. THC ranged from 5.9 to 2430.7 pg/mg; one sample had THC-OH above LLOQ (61.4 pg/mg); THC-COOH ranged from 0.3 and 36.4 pg/mg; CBN from 5.7 to 461.0 pg/mg; and CBD from 5.7 to 850.2 pg/mg. Results aligned with self-reported use, confirming the method's forensic suitability.