ABSTRACT
INTRODUCTION: Ayahuasca is a psychoactive drink originally consumed by indigenous people of the Amazon. The lack of regulation of this drink leads to uncontrolled consumption, and it is often consumed in religious contexts. OBJECTIVE: The aim of this work is to compare three miniaturised extraction techniques for extracting the main ayahuasca compounds from beverages. METHODOLOGY: Three sample pretreatment techniques were evaluated (dispersive liquid-liquid microextraction [DLLME], microextraction by packed sorbent [MEPS] and QuEChERS [Quick, Easy, Cheap, Effective, Rugged and Safe]) for the simultaneous extraction of N,N-dimethyltryptamine (DMT), tetrahydroharmine (THH), harmine, harmaline, harmol and harmalol from ayahuasca beverage samples. Then, the most promising technique (QuEChERS) was chosen to pre-concentrate the analytes, subsequently detected by high-performance liquid chromatography coupled to a diode array detector (HPLC-DAD). RESULTS: The procedure was optimised, with the final conditions being 500 µL of extractor solvent, 85 mg of primary secondary amine (PSA) and 4 s of vortexing. The analytical method was validated, showing to be linear between 0.16 and 10 µg/mL for ß-carbolines and between 0.016 and 1 µg/mL for DMT, with coefficients of determination (R2) between 0.9968 and 0.9993. The limit of detection (LOD) and lower limit of quantification (LLOQ) were 0.16 µg/mL for all compounds, except for DMT (0.016 µg/mL) and extraction efficiencies varied between 60.2% and 88.0%. CONCLUSION: The analytical methodology proved to be accurate and precise, with good linearity, LODs and LLOQs. This method has been fully validated and successfully applied to ayahuasca beverage samples.
Subject(s)
Banisteriopsis , Beverages , Liquid Phase Microextraction , Chromatography, High Pressure Liquid/methods , Banisteriopsis/chemistry , Beverages/analysis , Liquid Phase Microextraction/methods , Limit of Detection , Reproducibility of ResultsABSTRACT
This review emphasises the importance of opioid monitoring in clinical practice and advocates for a personalised approach based on pharmacogenetics. Beyond effectively managing pain, meticulous oversight is required to address concerns about side effects, specially due to opioid-crisis-related abuse and dependence. Various monitoring techniques, along with pharmacogenetic considerations, are critical for personalising treatment and optimising pain relief while reducing misuse and addiction risks. Future perspectives reveal both opportunities and challenges, with advances in analytical technologies holding promise for increasing monitoring efficiency. The integration of pharmacogenetics has the potential to transform pain management by allowing for a precise prediction of drug responses. Nevertheless, challenges such as prominent pharmacogenetic testing and guideline standardisation persist. Collaborative efforts are critical for transforming scientific advances into tangible improvements in patient care. Standardised protocols and interdisciplinary collaboration are required to ensure consistent and evidence-based opioid monitoring. Future research should look into the long-term effects of opioid therapy, as well as the impact of genetic factors on individual responses, to help guide personalised treatment plans and reduce adverse events. Lastly, embracing innovation and collaboration can improve the standard of care in chronic pain management by striking a balance between pain relief and patient safety.
Subject(s)
Analgesics, Opioid , Pain Management , Precision Medicine , Humans , Analgesics, Opioid/therapeutic use , Analgesics, Opioid/adverse effects , Precision Medicine/methods , Pain Management/methods , Drug Monitoring/methods , Chronic Pain/drug therapy , Pharmacogenetics/methods , Opioid-Related DisordersABSTRACT
Cannabis-based products have gained attention in recent years for their perceived therapeutic benefits (with cannabinoids such as THC and CBD) and widespread availability. However, these products often lack accurate labelling regarding their cannabinoid content. Our study, conducted with products available in Portugal, revealed significant discrepancies between label claims and actual cannabinoid compositions. A fully validated method was developed for the characterisation of different products acquired from pharmacies and street shops (beverages, herbal samples, oils, and cosmetic products) using high-performance liquid chromatography coupled with a diode array detector. Linearity ranged from 0.4 to 100 µg/mL (0.04-10 µg/mg) (THC, 8-THC, CBD, CBG, CBDA, CBGA), 0.1-100 µg/mL (0.01-10 µg/mg) (CBN), 0.4-250 µg/mL (0.04-25 µg/mg) (THCA-A), and 0.8-100 µg/mL (0.08-10 µg/mg) (CBCA). Among sampled beverages, none contained detectable cannabinoids, despite suggestive packaging. Similarly, oils often differed from the declared cannabinoid compositions, with some containing significantly higher CBD concentrations than labelled. These inconsistencies raise serious concerns regarding consumer safety and informed decision-making. Moreover, our findings underscore the need for stringent regulation and standardised testing protocols to ensure the accuracy and safety of cannabis-based products.
Subject(s)
Cannabinoids , Cannabis , Portugal , Cannabinoids/analysis , Cannabinoids/chemistry , Cannabis/chemistry , Chromatography, High Pressure Liquid , Humans , Cosmetics/analysis , Cosmetics/chemistry , Beverages/analysis , Medical Marijuana/analysis , Medical Marijuana/chemistryABSTRACT
Antipsychotics have narrow therapeutic windows, and their monitoring in biological fluids is therefore important; consequently, stability in those fluids must be investigated during method development and validation. This work evaluates the stability of chlorpromazine, levomepromazine, cyamemazine, clozapine, haloperidol, and quetiapine in oral fluid (OF) samples, using the dried saliva spots (DSS) sampling approach and gas chromatography coupled to tandem mass spectrometry. Since many parameters can influence the stability of the target analytes, design of experiments was adopted to check the crucial factors that affect that stability in a multivariate fashion. The studied parameters were the presence of preservatives at different concentrations, temperature, light, and time. It was possible to observe that antipsychotic stability improved when OF samples in DSS were stored at 4 °C, with a low ascorbic acid concentration, and in the absence of light. With these conditions, chlorpromazine and quetiapine were stable for 14 days, clozapine and haloperidol were stable for 28 days, levomepromazine remained stable for 44 days, and cyamemazine was stable for the entire monitored period (146 days). This is the first study that evaluates the stability of these antipsychotics in OF samples after application to DSS cards.
Subject(s)
Antipsychotic Agents , Clozapine , Quetiapine Fumarate , Haloperidol , Chlorpromazine , Methotrimeprazine/analysis , Gas Chromatography-Mass Spectrometry/methodsABSTRACT
Cannabis is the most consumed illicit drug worldwide, and its legal status is a source of concern. This study proposes a rapid procedure for the simultaneous quantification of Δ9-tetrahydrocannabinol (THC), 11-hydroxy-Δ9-tetrahydrocannabinol (11-OH-THC), 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THC-COOH), cannabidiol (CBD), and cannabinol (CBN) in urine samples. Microextraction by packed sorbent (MEPS) was used to pre-concentrate the analytes, which were detected by gas chromatography-mass spectrometry. The procedure was previously optimized, and the final conditions were: conditioning with 50 µL methanol and 50 µL of water, sample load with two draw-eject cycles, and washing with 310 µL of 0.1% formic acid in water with 5% isopropanol; the elution was made with 35 µL of 0.1% ammonium hydroxide in methanol. This fast extraction procedure allowed quantification in the ranges of 1-400 ng/mL for THC and CBD, 5-400 ng/mL for CBN and 11-OH-THC, and 10-400 ng/mL for THC-COOH with coefficients of determination higher than 0.99. The limits of quantification and detection were between 1 and 10 ng/mL using 0.25 mL of sample. The extraction efficiencies varied between 26 and 85%. This analytical method is the first allowing the for determination of cannabinoids in urine samples using MEPS, a fast, simple, and low-cost alternative to conventional techniques.
Subject(s)
Cannabidiol , Cannabinoids , Cannabidiol/analysis , Cannabinoids/analysis , Cannabinol/analysis , Dronabinol/analysis , Gas Chromatography-Mass Spectrometry/methods , Methanol/analysis , WaterABSTRACT
Drug abuse still represents a global problem, and it is associated with an increased risk of diseases, injuries, and deaths. Cocaine (COC) and opiates are the most abused drugs and account for a significant number of fatalities. Therefore, it is important to develop methods capable of effectively identifying and quantifying these substances. The present study aims to evaluate the long-term stability of COC, ecgonine methylester (EME), benzoylecgonine (BEG), cocaethylene (COET), norcocaine (NCOC), morphine (MOR), codeine (COD) and 6-monoacetylmorphine (6-MAM) in oral fluid samples. The analytes of interest were isolated from the matrix (50 µL) using the dried saliva spots (DSS) sampling approach and were subsequently analyzed by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). The parameters that could influence the stability of the target compounds were studied, and these were storage temperature, light, use of preservatives (and respective concentrations), and time. The effects of each parameter were evaluated using the design of experiments (DOE) approach. The stability of the target analytes was improved when the DSS were stored at room temperature, in the presence of light and using 1% sodium fluoride. The best conditions were then adopted for the DSS storage and long-term stability was assessed. COD was only stable for 1 day, EME was stable for 3 days, COC, COET, NCOC and 6-MAM were stable for 7 days, MOR for 14 days and BEG remained stable throughout the study (136 days). This is the first study that evaluates the stability of these compounds in oral fluid samples after application in DSS cards, and optimizes the conditions in order to improve their stability.
Subject(s)
Cocaine , Opiate Alkaloids , Cocaine/metabolism , Gas Chromatography-Mass Spectrometry/methods , Narcotics/analysis , Saliva/chemistry , Tandem Mass SpectrometryABSTRACT
Nanoparticles offer targeted delivery of drugs with minimal toxicity to surrounding healthy tissue and have great potential in the management of human papillomavirus (HPV)-related diseases. We synthesized lipid-modified AS1411 aptamers capable of forming nanoaggregates in solution containing Mg2+. The nanoaggregates presented suitable properties for pharmaceutical applications such as small size (100â¯nm), negative charge, and drug release. The nanoaggregates were loaded with acridine orange derivative C8 for its specific delivery into cervical cancer cell lines and HPV-positive tissue biopsies. This improved inhibition of HeLa proliferation and cell uptake without significantly affecting healthy cells. Finally, the nanoaggregates were incorporated in a gel formulation with promising tissue retention properties aiming at developing a local delivery strategy of the nanoaggregates in the female genital tract. Collectively, these findings suggest that the nanoformulation protocol has great potential for the delivery of both anticancer and antiviral agents, becoming a novel modality for cervical cancer management.
Subject(s)
Antineoplastic Agents , Antiviral Agents , Aptamers, Nucleotide , Cell Proliferation/drug effects , Drug Delivery Systems , Oligodeoxyribonucleotides , Uterine Cervical Neoplasms/drug therapy , Antineoplastic Agents/chemistry , Antineoplastic Agents/pharmacokinetics , Antineoplastic Agents/pharmacology , Antiviral Agents/chemistry , Antiviral Agents/pharmacokinetics , Antiviral Agents/pharmacology , Aptamers, Nucleotide/chemistry , Aptamers, Nucleotide/pharmacokinetics , Aptamers, Nucleotide/pharmacology , Female , HeLa Cells , Humans , Oligodeoxyribonucleotides/chemistry , Oligodeoxyribonucleotides/pharmacokinetics , Oligodeoxyribonucleotides/pharmacology , Uterine Cervical Neoplasms/metabolismABSTRACT
Ayahuasca is a psychoactive beverage that contains the psychoactive compound N,N-dimethyltryptamine and ß-carboline alkaloids. This study aims at determining in vitro the bioavailability and bioaccessibility of the main compounds present in decoctions of four individual plants, in a commercial mixture and in four mixtures of two individual plants used in the preparation of Ayahuasca. The samples were subjected to an in vitro digestion process, and the Caco-2 cell line was used as an absorption model. The integrity and permeability of the cell monolayer were evaluated, as well as the cytotoxicity of the extracts. After digestion and cell incubation, the compounds absorbed by the cell monolayer were quantified by high-performance liquid chromatography coupled to a diode array detector. The results showed that compounds such as N,N-dimethyltryptamine, Harmine, Harmaline, Harmol, Harmalol and Tetrahydroharmine were released from the matrix during the in vitro digestion process, becoming bioaccessible. Similarly, some of these compounds, after being incubated with the cell monolayer, were absorbed, becoming bioavailable. The extracts did not show cytotoxicity after cell incubation, and the integrity and permeability of the cell monolayer were not compromised.
Subject(s)
Banisteriopsis , Beverages/analysis , Biological Availability , Caco-2 Cells , Humans , N,N-DimethyltryptamineABSTRACT
Cocaine is still one of the most commonly used illicit substances worldwide, with an estimated 4 million users in Europe in the last year. Hair samples have been widely used for the determination of episodic or repeated consumption of this substance, but the use of miniaturized techniques for hair sample clean-up has been challenging due to the sample complexity. Despite hair's complex matrix, MEPS provides a method that is fast, reduces the volume of extraction solvents used, and offers low-cost options (since extraction beds may be reused several times). Microextraction by packed sorbent using a mixed-mode sorbent was optimized for hair sample clean-up in order to determine cocaine, benzoylecgonine, ecgonine methyl ester, norcocaine, cocaethylene and anhydroecgonine methyl ester by gas chromatography coupled to tandem mass spectrometry. The method was fully validated according to internationally accepted criteria, presenting good linearity between the limits of quantification (0.01-0.15) and 5 ng/mg. Precision and accuracy resulted in coefficients of variation typically lower than 15%, with mean relative errors within ±15% for all compounds, except for the limit of quantification (±20%). The present work describes the first application of microextraction by packed sorbent for the concentration of cocaine and metabolites extracted from hair samples. Graphical abstract.
Subject(s)
Cocaine/analysis , Hair/chemistry , Solid Phase Microextraction/methods , Cocaine/metabolism , Gas Chromatography-Mass Spectrometry/methods , Humans , Limit of Detection , Miniaturization , Reproducibility of ResultsABSTRACT
Julbernardia paniculata and Pterocarpus angolensis are two plant species with important application in African traditional medicine, particularly in Angola, in the treatment of several diseases. However, scientific studies concerning these species are scarce. The goal of this work was to know better which medicinal approaches are used by the Huíla population in Angola by means of ethnobotanical surveys. Furthermore, extracts of both plants were phytochemically characterized. Antioxidant, anti-inflammatory, wound-healing activities, and potential cytotoxicity were also studied. With this study it was possible to verify that 67% of the individuals that use medicinal plants are women, and their main therapeutic uses are the treatment of problems of the digestive system and skin disorders. Barks of J. paniculata and leaves of P. angolensis are the most often used plant parts. Through high-performance liquid chromatography coupled to diode-array detector (HPLC-DAD) and GC-MS it was possible to characterize the chemical composition of the two species, which are rich in phenolic compounds, terpenes, terpenoids, sesquiterpenoids and fatty acids. Both plants showed to possess antioxidant, anti-inflammatory proprieties, and wound-healing activity. To the best of our knowledge, this is the most comprehensive study of these two species and the first ethnobotanical and ethnopharmacological study of medicinal plants from this region of Angola.
Subject(s)
Anti-Inflammatory Agents/pharmacology , Antioxidants/pharmacology , Fabaceae/chemistry , Phytochemicals/pharmacology , Adult , Angola , Anti-Inflammatory Agents/isolation & purification , Antioxidants/isolation & purification , Cell Line , Chromatography, High Pressure Liquid , Ethnopharmacology , Fabaceae/classification , Female , Gas Chromatography-Mass Spectrometry , Humans , Male , Models, Biological , Phytochemicals/isolation & purification , Pterocarpus/chemistry , Wound Healing/drug effectsABSTRACT
Organophosphorus insecticides, such as parathion-ethyl, quinalphos, chlorpyrifos, chlorfenvinphos or diazinon, are still widely used for pest control on crops. These compounds are extremely toxic to humans, and, even though specific legislation exists that controls the use of these substances, the frequency of toxic and/or fatal events and the existing data suggest that they are still easily accessed and the knowledge associated to the risks is not well-recognized. For these reasons, the determination of the exposure to these compounds, their detection (and of their metabolites as well) in biological samples, is of great importance in clinical and forensic toxicology, and, therefore, the development of techniques for this evaluation is an important task for laboratories. Most confirmatory analyses use blood, serum, plasma and urine as biological samples and are performed by either gas chromatographic-mass spectrometric or liquid chromatographic-mass spectrometric instrumentation, which represents the gold standard in what concerns high sensitivity. This paper will not only address the physical-chemical and toxicological aspects of this class of compounds but also perform a comprehensive and critical review on the analytical methods available for their determination in biological specimens, with special focus on the latest instrumental developments and sample preparation approaches.
Subject(s)
Forensic Toxicology/methods , Organophosphate Poisoning/diagnosis , Pesticides/analysis , Chromatography, Liquid , Gas Chromatography-Mass Spectrometry , Gastrointestinal Contents/chemistry , Hair/chemistry , Humans , Kidney/chemistry , Liquid-Liquid Extraction , Liver/chemistry , Lung/chemistry , Molecular Structure , Myocardium/chemistry , Pesticides/pharmacokinetics , Pesticides/toxicity , Saliva/chemistry , Solid Phase ExtractionABSTRACT
The present work describes the development and validation of a novel approach to determine methadone (MTD) and its main metabolite (EDDP) in oral fluid samples, using the dried saliva spots (DSS) sampling approach and gas chromatography-tandem mass spectrometry (GC-MS/MS). Oral fluid samples (50 µL) were applied into Whatman™ 903 protein saver filter paper cards and were allowed to dry overnight. The extraction was carried out by immersion of the spot in 1 mL of isopropyl alcohol with agitation for 1 min. Afterwards, the extract was centrifuged for 15 min at 3500 rpm and the supernatant evaporated to dryness and reconstituted with 50 µL of methanol. The procedure was considered linear in the range of 10 to 250 ng/mL for both compounds, with determination coefficients greater than 0.99. Intra- and inter-day precision and accuracy revealed coefficients of variation (CVs) lower than 15% at the studied concentrations, with mean relative errors within ± 15% of the nominal concentrations. Recoveries ranged from 45 to 74%. The limits of detection and quantification were 5 and 10 ng/mL respectively for both analytes. All studied parameters complied with the defined criteria and the method enabled the successful determination of MTD and EDDP in oral fluid samples from patients undergoing opiate substitution/maintenance therapy.
Subject(s)
Analgesics, Opioid/pharmacokinetics , Drug Monitoring/methods , Gas Chromatography-Mass Spectrometry/methods , Methadone/pharmacokinetics , Pyrrolidines/pharmacokinetics , Saliva/metabolism , Analgesics, Opioid/analysis , Humans , Limit of Detection , Methadone/analysis , Pyrrolidines/analysis , Saliva/chemistry , Tandem Mass Spectrometry/methodsABSTRACT
The present work describes the optimization and validation of an analytical method for the determination of six antipsychotic drugs (chlorpromazine, levomepromazine, cyamemazine, clozapine, haloperidol, and quetiapine) in oral fluid samples after solvent extraction from dried saliva spots, by gas chromatography coupled to tandem mass spectrometry. The method was fully validated, and the included parameters were selectivity, linearity, limits of quantification, precision and accuracy, stability, and recovery. The method was linear for all compounds from 10 to 400 ng/mL, except for haloperidol (5-100 ng/mL), presenting coefficients of determination higher than 0.99. Inter- and intra-day precision and accuracy were in conformity with the criteria usually seen in bioanalytical method validation; i.e., coefficients of variation were lower than 15% and an accuracy of 15% or better for all studied drugs. The recoveries obtained with this miniaturized technique ranged from 63 to 97%. The herein described method is the first to be reported using the dried saliva spots approach for the analysis of these antypshychotic drugs, proving great sensitivity apart from its simple and fast procedure. The method was considered a good alternative to the conventional techniques to be applied in clinical and toxicological analyses, even more taking into account the extremely low sample volume used (50 µL). Graphical abstract.
Subject(s)
Antipsychotic Agents/analysis , Gas Chromatography-Mass Spectrometry/methods , Saliva/chemistry , Tandem Mass Spectrometry/methods , Desiccation , Equipment Design , Gas Chromatography-Mass Spectrometry/instrumentation , Humans , Limit of Detection , Tandem Mass Spectrometry/instrumentationABSTRACT
RATIONALE: Antipsychotic drugs are prescription medications used to treat psychotic disorders, such as schizophrenia, schizoaffective disorder, or psychotic depression. With several antipsychotic drugs currently available all over the world, this class of drugs has quickly gained importance in both the clinical and forensic context. This work describes the development and validation of a methodology for the determination of seven antipsychotic drugs in plasma and oral fluid samples. METHODS: The antipsychotic drugs (chlorpromazine, clozapine, haloperidol, olanzapine, quetiapine, cyamemazine and, levomepromazine) were isolated from 0.2 mL of oral fluid and 0.5 mL of plasma using solid-phase extraction (SPE) following analysis by gas chromatography/tandem mass spectrometry (GC/MS/MS). The method was validated according to the international guidelines in terms of selectivity, linearity, accuracy, precision and recovery. RESULTS: The procedure was linear within 2-600 ng/mL (plasma) and 2-400 ng/mL (oral fluid), the intervals varying according to the compound; a mean R2 value of 0.99 was obtained and the calibrator's accuracy (mean relative error) was within a ±15 % interval for all concentrations. The limits of detection ranged from 1 to 10 ng/mL. Within- and between-run precision and accuracy were acceptable for all studied compounds. The extraction efficiency of the process ranged from 79% to 95%. The method was applied to authentic specimens. CONCLUSIONS: The described method was proven selective and sensitive for the determination of antipsychotics in low sample volumes using SPE and GC/MS/MS. This method was considered suitable not only for routine analysis of patients undergoing antipsychotic treatment (to evaluate compliance), but also in forensic scenarios where the studied compounds may be involved. To the best of our knowledge, this is the first work that reports the determination of antipsychotic drugs in oral fluid using MS/MS.
Subject(s)
Antipsychotic Agents/chemistry , Gas Chromatography-Mass Spectrometry/methods , Saliva/chemistry , Antipsychotic Agents/blood , Antipsychotic Agents/isolation & purification , Clozapine/blood , Clozapine/chemistry , Humans , Phenothiazines/blood , Phenothiazines/chemistry , Plasma/chemistry , Solid Phase Extraction , Tandem Mass Spectrometry/methodsABSTRACT
This work describes the optimization of a new method for the determination of five organophosphorus insecticides in whole blood. The analytes were extracted from the matrix (50 µL) using the dried blood spot (DBS) approach and were analyzed by gas chromatography (GC) coupled to tandem mass spectrometry (MS/MS). The studied compounds (diazinon, chlorpyrifos, parathion-ethyl, chlorfenvinphos and quinalphos) were chosen based on the statistics of intoxications in Portugal, and ethion was used as internal standard. The method was fully validated, taking into account international guidelines for bioanalytical method validation, such as those of the Food and Drug Administration (FDA), International Conference on Harmonization (ICH) and Scientific Working Group for Forensic Toxicology (SWGTOX). A linear range of 0.1-25 µg/mL was obtained for all compounds, except for diazinon and quinalphos (0.05-25 µg/mL and 0.25-25 µg/mL, respectively), presenting determination coefficients above 0.99. Concerning precision, the coefficients of variation (CVs) were lower than 14% for all compounds. Those compounds were found to be stable in the samples. Although the values obtained for recovery were low (between 1 and 12%), the method proved to be sensitive, since detection limits between 0.05 and 0.1 µg/mL were obtained. The novelty is the use of the DBS approach in the extraction of these compounds, and this is the first paper reporting it: DBS is a recent technique of bioanalysis in the field of toxicology, and in addition to its simplicity and sensitivity, it is applicable routinely in both clinical and forensic toxicology situations. Graphical abstract á .
Subject(s)
Gas Chromatography-Mass Spectrometry/methods , Insecticides/blood , Organophosphonates/chemistry , Tandem Mass Spectrometry/methods , Dried Blood Spot Testing/methods , Humans , Insecticides/chemistry , Limit of Detection , Organophosphonates/blood , Specimen HandlingABSTRACT
Cocaine is still one of the most abused drugs worldwide and, as such, it is often screened for in driving-under-the-influence or workplace drug - testing scenarios. A large number of samples have usually to be processed in those situations, and this requires fast and simple extraction procedures for the detection and quantification of the drugs. The present work describes an ultrafast and fully validated procedure for the simultaneous detection and quantification of cocaine and its two main metabolites, ecgonine methyl ester and benzoylecgonine, in urine using microextraction by packed sorbent and GC-MS. A small sample volume (200 µL) was used, and a fast extraction procedure together with a microwave-assisted derivatization (800 W, 2 min) allowed the quantification of all analytes in a range of 25 to 1000 ng/mL (r 2 > 0.99). Inter-day precision revealed coefficients of variation (CVs) lower than 10% for all analytes at the tested concentration levels, with an accuracy within a ±7% interval, with the exception of EME's lowest calibrator (±17%). Intra-day CVs were lower than 15% at the studied concentration levels, with a mean relative error within a ±13% interval. Recoveries ranged from 14.5 to 37.2% (EME), 67.0 to 83.3% (cocaine), and 24.6 to 43.5% (BEG), allowing the limits of detection and quantification to be set at 25 ng/mL for all compounds. Graphical Abstract Schematized analysis of cocaine and metabolites in urine by MEPS- GC/MS.
Subject(s)
Cocaine/urine , Gas Chromatography-Mass Spectrometry/methods , Calibration , HumansABSTRACT
In recent years, the crucial role played by essential oils in various areas such as health, cosmetics, crop protection, and food industries has been increasingly recognized [...].
ABSTRACT
Several protocols for the analysis of amphetamine-type stimulants (ATS) in hair have been developed over the years, with microextraction by packed sorbent (MEPS) being used for drugs like opiates, cocaine and ketamine. However, concerning ATS determination in hair samples, this approach has only been applied so far to amphetamine (AMP) and methamphetamine (MAMP). This study aimed at developing and validating a MEPS-based procedure for the determination in hair of not only AMP and MAMP but also of 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), 1-(1,3-benzodioxol-5-yl)propan-2-yl (ethyl)amine (MDE) and N-methyl-1-(1,3-benzodioxol-5-yl)-2-aminobutane (MBDB) as well. Hair, 50 mg, was incubated with 1 M sodium hydroxide (NaOH) at 45°C overnight, neutralization with 10 M hydrochloric acid (HCl) and centrifugation followed. The design of experiments approach was used for MEPS optimization, with the final optimized conditions including conditioning (250 µL methanol and deionized water), loading (18 × 100 µL) and elution (7 × 100 µL 2% NH4OH in acetonitrile). The eluted extract was evaporated to dryness and underwent microwave-assisted derivatization with N-methyl-bis(trifluoroacetamide) (MBTFA), and it was afterwards injected onto the gas chromatography-mass spectrometer (GC-MS). The obtained recoveries ranged between 8% and 14% for AMP, 14% and 20% for MAMP, 10% and 15% for MDA, 18% and 28% for MDMA, 25% and 43% for MDE and 34% and 52% for MBDB, and the method was linear from 0.2 to 5.0 ng/mg. Precision and accuracy were in accordance with international method validation guidelines. This novel method involving MEPS coupled to GC-MS offers a swift, eco-friendly and cost-effective alternative to traditional procedures for detecting these AMPs in hair samples.
ABSTRACT
Therapeutic drug monitoring is an established practice for a small group of drugs, particularly those presenting narrow therapeutic windows, for which there is a direct relationship between concentration and pharmacological effects at the site of action. Drug concentrations in biological fluids are used, in addition to other clinical observation measures, to assess the patient's status, since they are the support for therapy individualization and allow assessing adherence to therapy. Monitoring these drug classes is of great importance, as it minimizes the risk of medical interactions, as well as toxic effects. In addition, the quantification of these drugs through routine toxicological tests and the development of new monitoring methodologies are extremely relevant for public health and for the well-being of the patient, and it has implications in clinical and forensic situations. In this sense, the use of new extraction procedures that employ smaller volumes of sample and organic solvents, therefore considered miniaturized and green techniques, is of great interest in this field. From these, the use of fabric-phase extractions seems appealing. Noteworthy is the fact that SPME, which was the first of these miniaturized approaches to be used in the early '90s, is still the most used solventless procedure, providing solid and sound results. The main goal of this paper is to perform a critical review of sample preparation techniques based on solid-phase microextraction for drug detection in therapeutic monitoring situations.
ABSTRACT
This review delves into the therapeutic applications of amphetamine-type stimulants such as lisdexamphetamine dimesylate, mixed amphetamine salts, 3,4-methylenedioxymethamphetamine (MDMA), dextroamphetamine, and phentermine. These compounds have been investigated for their potential in treating a range of psychiatric disorders, including attention deficit hyperactivity disorder (ADHD), drug dependence, post-traumatic stress disorder (PTSD), and obesity. Lisdexamphetamine dimesylate has shown promise in effectively treating ADHD symptoms in both children and adults. Additionally, it has been explored as a potential treatment for drug dependency and withdrawal, demonstrating encouraging results. Mixed amphetamine salts have also exhibited efficacy in reducing ADHD symptoms in adults. Future research should explore their potential use in treating bipolar disorder and cocaine dependence, considering the associated risks and benefits. MDMA-assisted psychotherapy has emerged as an innovative approach to treating PTSD, leading to sustained reductions in symptoms and even promoting post-traumatic growth. Furthermore, it has shown promise in managing anxiety related to life-threatening illnesses. Dextroamphetamine and phentermine have demonstrated efficacy in treating cocaine and opioid dependence, ADHD, and obesity. However, careful consideration and monitoring by medical professionals are essential due to the potential risks and benefits associated with them. In conclusion, amphetamine-type stimulants present a promising avenue for therapeutic interventions in various psychiatric conditions. Nevertheless, further research is necessary to comprehensively understand their mechanisms of action, dosage requirements, and long-term effects in different patient populations.