Drug Testing and Analysis最新文献

This study evaluates the methamphetamine contamination routes through exposure to sweat, smoke in the environment and direct contact, as well as the effectiveness of decontamination procedures. For sweat exposure, drug-free hair samples (n = 10) were sprayed with artificial sweat containing amphetamine and methamphetamine at either ‘low’ (2.6 and 6.5 ng/mL, respectively) or ‘high’ concentration (3.1 and 25.2 ng/mL, respectively), 5 times (2 mL each time) per day for 5 days. In the smoke exposure, 2 mg of methamphetamine hydrochloride powder was heated and vapourised on one side of an enclosed cardboard box containing hair (n = 10) on the other side. In the direct contact with methamphetamine powder, 0.6 mg of methamphetamine hydrochloride was rubbed gently by hand onto hair (n = 5) for 1 min. Each contaminated hair sample was then subjected to either one of the 3 wash methods, namely, (1) sequential wash using dichloromethane, water, and methanol; (2) sequential wash by hexane and acetone; and (3) methanol wash only. All solvents and hair samples were analysed. The results show that it was relatively difficult to remove methamphetamine from the hair that was exposed to methamphetamine in artificial sweat, followed by methamphetamine smoke and then direct contact with the methamphetamine powder. None of the wash methods was able to completely remove amphetamine and methamphetamine from the contaminated hair. Overall, methods (1) and (3) show better decontamination efficacy than method (2), probably due to the polar protic nature of the solvents.

S42, 4-Methyl-19-norpregna-1,3,5(10)-trien-20-one a new 20-keto-steroid, is a novel selective androgen receptor modulator (SARM). The World Anti-Doping Agency (WADA) bans the use of SARMs in sports at all times. In preparation of a sensitive detection procedure to control for S42 abuse, in vitro metabolism experiments were conducted and biotransformation products were analyzed with GC-EI MS-orbitrap instrumentation. S42-C20-OH, S42-C6ß-OH, and S42-C7α-OH were synthesized as reference material to study their exemplary EI-HR (electron ionization- high resolution) mass spectra. Additionally, S42-d7, synthesized earlier with ²H-labels at carbon atoms C1, C2, C3, C6, and C7, was used for the in vitro metabolism study. Comparison of the respective mass spectra of labeled and unlabeled reference materials and of specifically mass-shifted fragment ions provided the foundation for the structure elucidation of S42 in vitro phase I metabolites. Molecular ions of selected S42 phase I metabolites found in the in vitro experiments were submitted to higher energy collisional dissociation (HCD) MS²-product ion experiments to allow straightforward and secured assignment and interpretation of fragmentation patterns. At least eight phase I metabolites of S42 were identified in the in vitro study and analyzed as tri-methyl-silyl ether derivatives. Specifically, different singly, doubly, and triply hydroxylated metabolites of S42 were identified and analyzed with GC-EI HR MS.

Testosterone (T) formulations that are used for doping purposes often contain the steroid in esterified forms. As these esters are hydrolysed in the bloodstream before renal excretion, they can be detected in blood matrices and have not been detected in urine so far. Serum samples can additionally be used for longitudinal blood steroid profiling, but their collection, shipping and storage have some disadvantages. The use of dried blood spots (DBS), an alternative blood matrix, is more convenient for pre-analytical and post-analytical aspects but is not fully established in antidoping laboratories yet. To evaluate the ability of multiple antidoping laboratories to detect T-esters in serum and DBS samples, an interlaboratory study was organised. Common T-esters were spiked in five samples of each matrix (serum, cellulose card DBS, polymeric DBS) at concentrations that correspond to an administration scenario and sent as blinded specimens to each laboratory. The laboratories were requested to apply their own analytical method to detect the T-esters and to provide a rough estimate of their concentrations. All laboratories identified the spiked testosterone esters correctly in all samples and the estimated concentrations were deemed comparable (average relative standard deviation < 30%), considering that only qualitative initial testing procedures (ITPs) were used. This study could firstly demonstrate the capability of different analytical approaches to analyse T-esters in serum and DBS samples and, secondly, show that the methods employed by the participating laboratories are all fit for purpose.

2-Hydroxyethyl salicylate (2HES), a nonsteroidal anti-inflammatory drug (NSAID), is a medication to treat musculoskeletal injuries and inflammation swelling of humans and horses. Its misuse could affect the performance of horses and mask injuries, which could pose significant health risks. In horseracing, it is reported as an adverse finding once detected in competition. The metabolism of 2HES in either human or horse has not been reported, and therefore, little is known about its metabolic fate. This paper describes the in vivo metabolism of 2HES in horse with an objective to identify the most appropriate target(s) for detecting 2HES administration. To study the elimination and biotransformation of 2HES, topical administrations were performed by giving three castrated horses (geldings) each a total of 100-g Tensolvet gel (equivalent to 5 g of 2HES). The postulated in vivo metabolites included glucuronide-conjugated 2HES (2HES-Glu) and sulphate-conjugated 2HES (2HES-SO₄) from Phase II conjugation possibly at hydroxyethyl moiety and salicylic acid (SA) from hydrolysis of 2HES. To control the misuse of 2HES in horses effectively, 2HES was found to be the most suitable target. Total 2HES could be detected for up to 10 days in urine, whereas free 2HES could be detected for 16 h in plasma. As the maximum concentration of SA in postadministration urine and plasma sample did not exceed its corresponding international thresholds, monitoring the amount of SA could not be used as an indicator for possible 2HES exposure.

Since 2021, products claiming to contain Δ⁹-tetrahydrocannabinol (Δ⁹-THC) analogs have been distributed online and in physical stores, including liquid cartridges for electronic cigarettes, herbal products, and gummy products. This study identified the ingredients in products claiming to contain THC analogs distributed online. Seven oil products and one herbal product were analyzed via gas chromatography–mass spectrometry (GC–MS) and liquid chromatography–photodiode array–mass spectrometry (LC–PDA–MS). After isolating and purifying the unknown components from the products, structural analysis was performed by measuring ¹H and ¹³C nuclear magnetic resonance (NMR) spectroscopy and various two-dimensional NMR (COSY, HMQC, HMBC, and NOESY). The analysis revealed the presence of Δ⁸-tetrahydrocannabinol acetate (Δ⁸-THC-O), Δ⁹-tetrahydrocannabinol acetate (Δ⁹-THC-O), Δ⁴⁽⁸⁾-iso-THC-O-acetate, Δ⁹-tetrahydrocannabihexol acetate (Δ⁹-THCH-O), Δ⁹-tetrahydrocannabiphorol acetate (Δ⁹-THCP-O), Δ⁸-THC-O-propionate, Δ⁹-THC-O-propionate, Δ⁴⁽⁸⁾-iso-THC-O-propionate, Δ⁹-THCB-O-butanoate, and Δ⁹-THCP-O-butanoate in these products.

We present a case report of an adverse analytical finding (AAF) with suspected doping in an athlete following consumption of a supplement contaminated with Roxadustat, an oral inhibitor of hypoxia-inducible factor prolyl hydroxylase (HIP-PH), which increases erythropoietin production under normoxic conditions. Simultaneously, the athlete biological passport (ABP) profile was reviewed by experts of the World Anti-Doping Agency (WADA) ABP review panel and considered to be atypical and suspect of blood doping. A particular genetic testing was performed, which determined that this athlete had various reasons for fluctuations in her hematological parameters, such as the C677T and 1298C MTHFR mutations leading to chronic folate deficiency which can participate in the development of multiple hormonal and metabolic disturbances, heterozygous missense variant EPAS1 c.1292T>C, p. (Ile431Thr) and a heterozygous missense variant PIEZO1 c.7478T>G, p. (Leu2493Arg), both of which are variants of uncertain significance. This example illustrates the caution required when interpreting an ABP.

The use of transdermal patches, primarily for pain relief, has grown significantly in recent years. This increase in legitimate use has been accompanied by a rise in their illegal use. Consequently, forensic laboratories are facing a growing number of these complex samples requiring analysis. These systems often involve complex sample matrices, demanding analytical techniques that are both efficient and highly sensitive. This study introduces the application of QuickProbe GC–MS for the rapid identification of fentanyl and buprenorphine in transdermal patches. Utilizing in situ extraction, the method eliminates the need for time-consuming sample preparation, achieving a full analysis cycle time of under 2 min. QP GC–MS successfully detected fentanyl and buprenorphine at concentrations as low as 4.125 and 5 mg, respectively, while adhering to the highest selectivity guidelines. This rapid and streamlined approach has broader implications for forensic investigations, enabling high-throughput screening of seized drug samples and potentially extending to the analysis of emerging drugs of abuse. The speed and efficiency of QP GC–MS make it a valuable tool for law enforcement, public health agencies, and toxicology labs facing the challenge of keeping pace with evolving drug trends.