Drug Testing and Analysis

Doping analyses are essential for sporting events because some athletes might use prohibited substances to win games. To obtain reliable results from doping analyses, it is important to use both reliable standard solutions and validated analytical methods at accredited laboratories. Among the focused compounds related to prohibited substances listed by the World Anti-Doping Agency, we developed a certified reference material (CRM) for 3β,4α-dihydroxy-5α-androstan-17-one (DHAS), a metabolite of formestane that is used to conceal prohibited anabolic steroids, in methanol solution (NMIJ CRM 6212-a)...

Methadone has two enantiomers, which exhibit differences in pharmacological effects, with R-methadone being the active and S-methadone the inactive enantiomer. A robust, simple and rapid method for chiral separation of the two enantiomers in serum samples using ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MSMS) has been developed and validated. Enantiomeric separation was achieved using a Chiralpak IH-3 column with a mobile phase consisting of CO2 and 30mM ammonium acetate in methanol/water (98/2, v/v)...

This study evaluated an alternative routine for reporting urinary chiral amphetamine results in assessment of attention-deficit/hyperactivity disorder (ADHD) treatment with amphetamine medications and for detecting side-use of illicit racemic amphetamine. Currently in Sweden, only enantiopure d-amphetamine-based ADHD medications (lisdexamphetamine dimesylate and dexamphetamine sulfate) are approved. It is therefore unsuitable to express the chiral result as the l/d-ratio, as before, because l-amphetamine should not be present provided treatment compliance...

Latent fingerprints at crime scenes are frequently recovered using forensic gel-lifters, which can help to preserve the crime scene and to enhance visualisation of traces such as blood or paint. In addition to providing fingerprint ridge detail, additional chemical information can also be recovered from gel lifts that may prove pertinent to an investigation. However, while DNA and metal ions have been shown to be able to be detected in gel-lifted fingerprints, the determination of other types of chemical information such as the presence of drugs in gel-lifted prints has not been previously shown...

Drug overdoses have risen dramatically in recent years. We developed a simple nontargeted method using a disposable paper spray cartridge with an integrated solid phase extraction column. This method was used to screen for ~160 fentanyl analogs, synthetic cannabinoids, other synthetic drugs, and traditional drugs of abuse in over 300 authentic overdose samples collected at emergency departments in Indianapolis. A solid phase extraction step was implemented on the paper spray cartridge to enable subnanograms per milliliter synthetic drugs screening in plasma...

Areca nut (AN) is a carcinogen; its chewing cessation is, therefore, of worldwide interest. However, cessation biomarkers are lacking. We sought to establish arecoline in chewers' buccal cells (BCs) as a biomarker for AN dose. Self-reported AN doses, expressed as the average AN load ("AANL"), the product of AN amount, chewing time, and chewing frequency, were correlated by regression analysis with chewers' BC arecoline, measured by liquid chromatography mass spectrometry. We then determined whether associations differed between Class 1 chewers (who consume AN alone or with slaked lime, leaf, and/or spices) and Class 2 chewers (who consume any combination of the aforementioned ingredients plus tobacco)...

Α sensitive and selective derivatization and inject method for the quantification of intact nandrolone phase II oxo-metabolites was developed and validated using liquid chromatography - (tandem high resolution) mass spectrometry (LC-MS/(HRMS)). For the derivatization, Girard's reagent T (GRT) was used directly in natural urine samples and the analysis of the metabolites of interest was performed by direct injection into LC-MS/(HRMS) system operating in positive ionization mode. Derivatization enabled the efficient detection of nandrolone oxo-metabolites, while at the same time producing intense product ions under collision-induced dissociation (CID) conditions that are related to metabolites of the steroid backbone and not to the conjugated moieties...

Interpretation results of hair analysis, particularly for cocaine, can be challenging due to the need to differentiate between active use or passive contamination. Our study aimed to assess the impact of varying degrees of passive cocaine exposure hair analysis results and their interpretation. Hair samples (n = 25) were categorized based on the declared cocaine exposure of volunteers: (a) high, involving handling up to several kilograms of cocaine powder from dismantling illegal distribution sites; (b) medium, where staff dealt with cocaine blocks (up to kilograms); and (c) low, with staff in contact with up to grams of cocaine for laboratory analysis...

1-Acetyl-N,N-diethyllysergamide (1A-LSD, ALD-52) was first synthesized in the 1950s and found to produce psychedelic effects similar to those of LSD. Evidence suggests that ALD-52 serves as a prodrug in vivo and hydrolysis to LSD is likely responsible for its activity. Extension of the N1 -alkylcarbonyl chain gives rise to novel lysergamides, which spurred further investigations into their structure-activity relationships. At the same time, ALD-52 and numerous homologues have emerged as recreational drugs ("research chemicals") that are available from online vendors...

Wastewater-based epidemiology was applied in northeastern Brazil during a dance festival, revealing that cocaine consumption doubled during the event days. The daily drug loads were 0.95 ± 0.03 to 11.4 ± 0.4 g/day for BE, 1.8 ± 0.4 to 7.6 ± 0.3 g/day for COC, 0.04 ± 0.02 to 0.19 ± 0.02 g/day for COE, and 0.08 ± 0.02 to 0.80 ± 0.02 g/day for MDMA.

Estra-4,9-diene-3,17-dione (dienedione) is an anabolic androgenic steroid (AAS) sold as a bodybuilding supplement. It is prohibited in both human and equine sports. With no report of 4,9-diene configuration in endogenous steroids, dienedione has long been considered a synthetic AAS. Nevertheless, the reoccurring detection of dienedione in colt (entire male horse) urine samples lead to the investigation of its possible endogenous nature in horses. This paper describes (i) the detection of naturally occurring dienedione in colts, (ii) the conjugation study of dienedione and (iii) the population study of free and glucuronide-conjugated dienedione in colt urine...

Hair analysis plays an important role in the determination of drugs of abuse in both forensic and clinical toxicology investigations. The analysis of different substances often requires the use of different sample preparation methods, thereby increasing the amount of hair sample and time required. In the present study, a fast method involving a combination of a single 25 mg hair extraction procedure and four liquid chromatography-tandem mass spectrometry methods using the same chromatographic phases and column was developed and validated...

Testosterone, nandrolone, and boldenone, which are listed as doping substances on the World Anti-Doping Agency Prohibited List, are mostly available commercially in esterified forms. Isotope ratio mass spectrometry (IRMS) represents a key tool for identifying these substances, as they are hydrolyzed and discharged in the urine as pseudo-endogenous substances. However, IRMS, which comprises a complicated process, cannot achieve the direct detection of steroid esters in blood samples. These substances can be detected using dried blood spots (DBSs), reducing the impact of esterase hydrolysis...

As negative drug tests are frequently a condition for employment, some people who use drugs will try to subvert the testing. In this study, systematic web monitoring was used to investigate how drug test subversion is discussed online. Posts pertaining to drug test subversion were obtained from public websites and the dark web (n = 634, July-December 2021). Most information from public websites came from Twitter (65%), and 94% of dark web posts were from Reddit. The posts were manually coded to extract quantitative and qualitative information about drug test subversion tactics...

As gamma-hydroxybutyric acid (GHB) underlies fast metabolization, its determination from hair may presumably offer a detection window superior to that of body fluids. Due to the wide range of endogenous concentration levels, the evidence of an exogenous ingestion is challenging. As already shown for other drugs, the temporal resolution obtained by applying single hair microanalysis provides further information. Therefore, a method for the extraction and quantification of GHB in 2-mm hair segments (seg) was optimized and validated (limit of detection [LOD]: 2...

Infant exposure to drugs of abuse represents a worldwide problem whose extent is difficult to estimate. Despite the potentially serious health consequences, few data concerning exposure in children under 1 year of age are available. Since in clinical and forensic settings, neonatal and infant hair testing represents a useful method for investigating suspected drug exposures, an observational retrospective study was performed on hair analysis of children under 1 year of age evaluated at the University Hospital of Padova between 2018 and 2022 with the aim of estimate the extent and define the characteristics of this phenomenon in the reference setting...

The use of performance-enhancing substances not only undermines the core values of sports but also poses significant health risks to athletes. In a fast-evolving doping environment, where sport professionals are constantly seeking novel and illegal means to bypass doping tests, and new substances are regularly detected on the drug market, it is crucial to inform authorities with updated evidence emerging from scientific research. The current study aims to (i) outline the structure of knowledge in the literature on performance enhancers in sports (i...

5F-MDMB-PICA, an indole-type synthetic cannabinoid (SC), was classified illicit globally in 2020. Although the extensive metabolism of 5F-MDMB-PICA in the human body warrants the development of robust analytical methods for metabolite detection and quantification, a current lack of reference standards for characteristic metabolites hinders such method creation. This work described the synthesis of 18 reference standards for 5F-MDMB-PICA and its possible Phase I metabolites, including three hydroxylated positional isomers R14 to R16...

Vitamin D3 , an essential micronutrient, often requires supplementation via medicines or food supplements, which necessitate quality control (QC). This study presents the development of a method for detecting and quantifying seven impurities of vitamin D3 in oily drug products using supercritical fluid chromatography-mass spectrometry (SFC-MS). Targeted impurities include two esters of vitamin D3 and five non-esters including four that are isobaric to vitamin D3 . Firstly, a screening study highlighted the Torus 1-AA column and acetonitrile modifier as adequate for the separation, followed by optimization of the SFC conditions...

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