Drug Testing and Analysis

Globally, the number of drug users and the proportion of the drug using population has increased from 210 million in 2009 to 269 million in 2019. Several studies suggest that music festival attendees are more likely to abuse illicit substances and have a high-risk profile. Consequently, it is crucial to develop robust field drug analysis methods that facilitate harm reduction and drug monitoring. The work presented in this report aimed at developing and validating qualitative analytical methods for 3,4-methylenedioxymethamphetamine, 4-bromo-2,5-dimethoxyphenethylamine (2C-B), ketamine and N-ethylpentylone on two portable gas chromatography-mass spectrometry (GC-MS) systems: Griffin G510 (Teledyne FLIR, West Lafayette, IN) and Torion T-9 (PerkinElmer, Shelton, CT)...

The EPO gene variant, c.577del (VAR-EPO), was discovered in the Chinese population in 2021. The mutated protein is naturally present in urine from individuals heterozygous for the variant. Electrophoresis methods currently applied in anti-doping laboratories produce a pattern in samples from individuals carrying VAR-EPO that cannot be unambiguously distinguished from individuals who received recombinant EPO doses. Consequently, the analysis of blood samples is obligatory to facilitate interpretation of suspicious findings from urine samples...

Analysis of hair collected from putrefied or skeletal bodies is always complex and must take into account several pitfalls, such as external contamination and contamination by biological fluids. This work presents a case of particular complexity. A skeletonized body was discovered on a country road. A tuft of brown hair, detached from the scalp, irregular in length, non-oriented, in contact with soil and vegetation, was removed. An anthropological examination was carried out and genetic samples were taken from the right femoral shaft...

Methandienone is an anabolic-androgenic steroid that is prohibited in equine sports due to its potential performance enhancing properties. Metabolism and detection of methandienone in equine urine have been investigated comprehensively in literature; however, there is a limited knowledge about its metabolites in equine plasma and no information about its detection in equine hair. Following a multi-dose oral administration of methandienone to two Thoroughbred horses, 17-epimethandienone, methyltestosterone, two mono-hydroxylated, two di-hydroxylated and three 17α-methylandrostanetriol metabolites were detected in plasma...

As cannabidiol (CBD) is not considered to be a drug and because of its potential health claims, it is an interesting compound that is often found in cosmetics. However, the safety of CBD, as well as the presence of trace amounts of other phytocannabinoids, including the psychoactive substance ∆9 -tetrahydrocannabinol (THC), is still being debated. A robust analytical technique capable of analysing cosmetic products and determining their phytocannabinoid content will be crucial in assessing the safety of these products...

The proposed ICH Q14 guideline "Analytical procedure development" describes science and risk-based approaches for development and maintenance of analytical procedures suitable for the assessment of the quality of drug substances and drug products. As a case study, the systematic development and validation of a supercritical fluid chromatography (SFC)-based purity method for carbamazepine is presented. Systematic analytical quality by design (AQbD) principles were applied using the software package Fusion QbD to the method development approach...

A dopamine reuptake inhibitor is a type of medication or substance that works by blocking the reuptake of dopamine in the brain. Dopamine reuptake inhibitors offer multiple effects, including increased alertness, improved mood, and therapeutic potential for conditions like depression, ADHD, and Parkinson's disease. HDMP-28, or methylnaphthidate, is a potent synthetic stimulant from the phenyltropane class. It surpasses methylphenidate in both dopamine reuptake inhibition and half-life. As a dopamine reuptake inhibitor, it boosts dopamine levels by hindering reuptake into nerve cells, resulting in heightened stimulation and increased energy...

FG-4592 is a hypoxia-inducible factor inhibitor that has been approved for therapeutic use in some countries. This class of compounds can increase the oxygen carrying capacity of the blood and thus have the potential to be used as performance enhancing agents in sports. The purpose of this study was to investigate the detection of FG-4592 and metabolites in equine plasma and mane hair following a multiple dose oral administration to two Thoroughbred racehorses, to identify the best analytical targets for doping control laboratories...

Drug checking is a harm reduction measure that provides people with the opportunity to confirm the identity and purity of substances before consumption. The CanTEST Health and Drug Checking Service is Australia's first fixed-site drug checking service, where clients can learn about the contents of the samples they provide while receiving tailored harm reduction and health advice. Three samples were recently presented to the service with the expectation of 4-fluoromethylphenidate (4F-MPH) 1, methoxetamine (MXE) 2 and 3-methylmethcathinone (3-MMC) 3...

For antidoping laboratories, the determination of an illicit testosterone (T) administration in urine samples remains a difficult process as it requires the determination of the exogenous origin by carbon isotope ratios (CIRs) of testosterone and its metabolites. As a complement to the urinary analysis, targeting testosterone esters (e.g. testosterone undecanoate [TU]) in serum samples by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) could represent a simpler approach compared with isotope ratio mass spectrometry (IRMS)...

Methamphetamine is the illicit stimulant of choice in Australia. Countless initiatives have been employed to reduce methamphetamine use and drug-related harm. Wastewater analysis (WWA) has been used effectively as an objective measure of drug use at a population level and can be compared to indicators of harm, such as the number of drug-related fatalities. This paper attempts to describe methamphetamine use in the context of changes in levels measured in wastewater in South Australia whilst recognising considerable interventions over an 8-year period...

Adsorbents play a significant role in enhancing the analytical sensitivity of target analytes in complex samples by mitigating matrix effects. In our recent report, ZnO stood out among various adsorbents to determine target therapeutic drugs in complex biological matrices when applied for portable paper-based electrospray ionization mass spectrometry (PPESI-MS). However, the influence of the morphology of ZnO on the performance of PPESI-MS is elusive. Herein, different morphologies of ZnO particles were prepared via co-precipitation or ultrasonic methods, and their capability to determine different therapeutic drugs in serum were systemically investigated...

Δ9 -Tetrahydrocannabinol (Δ9 -THC) is usually the primary psychoactive agent in cannabis preparations. Recently, products containing another isomer, Δ8 -tetrahydrocannabinol (Δ8 -THC), have become available for sale. Δ8 -THC exists naturally in the cannabis plant at very low concentrations; hence, the Δ8 -THC present in most of the above-mentioned products is likely to be manufactured synthetically. A surge in popularity of these products, coupled with little oversight to ensure purity and potency, has led to reports of adverse events...

A multi-analyte liquid chromatography-tandem mass spectrometry (LC-MS/MS) method is described, involving the separation of delta-9-tetrahydrocannabinol (delta-9-THC) and delta-8-THC in addition to other commonly encountered drugs and metabolites. Briefly, sample preparation involved an alkaline liquid-liquid extraction (methyl tert-butyl ether) of blood (100 μl). The solvent layer was transferred, evaporated to dryness, reconstituted, and samples then separated on an Agilent Poroshell 120 EC-C18 100 Å (50 mm × 3...

Since 2016, illicitly manufactured fentanyls and fentanyl analogs (referred to as IMFs) have contributed to an increase in drug overdoses. Although fentanyl has been characterized and evaluated extensively in animals and humans, many of the clandestinely synthesized analogs of fentanyl have not and users may unknowingly ingest these IMFs leading to overdose and potentially death. The pharmacodynamic (PD) and pharmacokinetic (PK) properties of four IMFs and fentanyl were evaluated in Sprague-Dawley rats. A 300-μg/kg subcutaneous dose of each compound (fentanyl, acetylfentanyl, cyclopropylfentanyl, butyrylfentanyl, and valerylfentanyl) was given...

Forensic analysis can encompass a wide variety of analytes from biological samples including DNA, blood, serum, and fingerprints to synthetic samples like drugs and explosives. In order to analyze this variety, there are various sample preparation techniques, which can be time-consuming and require multiple analytical instruments. With recent advancements in ambient ionization mass spectrometry (MS), plasma-based dielectric barrier discharge ionization (DBDI) sources have demonstrated to cover a wide range of these analytes...

External contamination of hair by cannabis smoking requires a careful evaluation in forensic toxicology. Medical and recreational cannabis are increasingly consumed by e-cigarettes, which give rise to side-stream vapor. Moreover, products containing low Δ9-tetrahydrocannabinol (Δ9-THC) and rich in cannabidiol (CBD) started spreading legally. The goal of the present study was to assess whether hair analysis could allow to distinguish the type of delivered product, with low or high Δ9-THC, and the delivering mode, by smoking or vaping...

The ability to detect newly emerging substances is of great importance in reducing harms for people who use drugs. New psychoactive substances including novel benzodiazepines in the illicit drug supply have been linked to high rates of overdose deaths while complicating drug checking as an overdose prevention strategy. Paper-spray mass spectrometry (PS-MS) has emerged as a novel strategy to rapidly detect trace components in street drug samples. While targeted, low-resolution PS-MS methods have proven effective, newly emerging substances are often missed...

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Detection of doping with steroids that are also endogenous in the horse can be challenging, and a variety of approaches to distinguish exogenous administration from their natural presence are employed. Knowledge of endogenous concentrations of various steroids in different genders of horses (intact male, castrated male and female) and factors that could naturally affect them is beneficial for establishing ways for detection of their use. The current internationally adopted approaches include concentration-based thresholds in urine and plasma, steroid ratios in urine and targeting the administered intact steroid esters in plasma and hair...