Drug Test Anal [JOURNAL]
Sun
200 papers
Evaluation of Therapeutic Opioids in Hair of Neonatal and Pediatric Patients.
Polke M, Zapf F, Restin T … +2 more , Kraemer T, Binz TM
Drug Test Anal · 2025 Nov · PMID 40717173 · Full text
Forensic hair analysis poses a valuable tool for assessing opioid exposure in children and neonates. However, reliable literature data on opioid concentrations in the hair of this population are mostly scarce, making the...
Forensic hair analysis poses a valuable tool for assessing opioid exposure in children and neonates. However, reliable literature data on opioid concentrations in the hair of this population are mostly scarce, making the interpretation of such hair analysis results rather challenging. This noninterventional study aims to address this issue by investigating 118 hair samples of pediatric patients (median age: 50 days) from the University Children's Hospital Zurich. These patients were treated with medically approved novel synthetic opioids (fentanyl, remifentanil, sufentanil, or alfentanil) and traditional opioids (morphine, methadone, and hydromorphone) during their clinical treatment. Quantification of the opioids and selected metabolites was achieved by a previously validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) based method, which showed good sensitivity with lower limits of quantification (LLOQs) ranging from 0.1 to 1 pg/mg hair. Most analytes were successfully detected in patients' hair, with the majority being identified for the first time in this matrix. Significant correlations were found between the opioid concentrations in hair and the administered medication doses, indicating that hair analysis may reflect the extent of opioid exposure in this population. Furthermore, metabolite ratios similar to the ones commonly found in adult hair were identified, which are forensically important to differentiate between active intake of a drug and contamination. The metabolite ratio of β-hydroxyfentanyl to fentanyl was particularly well suited for children and neonatal patients. In conclusion, concentration ranges, metabolite ratios, and dose correlations of the studied opioids in pediatric hair were established, providing insights into opioid incorporation pathways.
Evaluation of Two Spectroscopic Techniques to Estimate the MDMA Dose of Ecstasy-Like Tablets, an On-Site Approach.
Meert N, Segers K, Van Durme F … +1 more , Eliaerts J
Drug Test Anal · 2025 Nov · PMID 40695467 · Publisher ↗
MDMA, commonly known as "ecstasy," is widely used in clubs and at festivals, earning its reputation as a "party drug." The increasing demand for rapid on-site dose estimation of MDMA in tablets arises from the need of va...
MDMA, commonly known as "ecstasy," is widely used in clubs and at festivals, earning its reputation as a "party drug." The increasing demand for rapid on-site dose estimation of MDMA in tablets arises from the need of various stakeholders, including law enforcement, emergency services, and public health officials, to respond appropriately to potential public safety risks and incidents. This study evaluates the performance of two portable spectroscopic techniques (near-infrared [NIR] and Fourier-transform-infrared [FT-IR]) combined with chemometric modelling for estimating the MDMA dose in tablets. Ninety-eight seized tablets were measured on-site with both spectroscopic techniques and confirmed by the reference techniques: gas chromatography (GC) combined with a mass spectrometer (MS) and a flame-ionization detector (FID). Considering the correlation values (NIR: R = 0.64 for indirect contact with intact tablets, 0.87 for direct contact with homogenized tablets; FT-IR: R = 0.84) and the RMSEP values (NIR: 8.0 for indirect contact with intact tablets, 5.9 for direct contact with homogenized tablets; FT-IR: 5.4), both spectroscopic techniques provide a reliable dose prediction in comparison to the GC-FID results. Moreover, these devices are suitable for rapid on-site application. The instruments' choice depends on several factors, such as speed, safety measures, and laboratory support for modelling. However, determining the MDMA dose does not address all health risks. Other factors, such as the presence of low-dosed substances (undetectable on-site) and the combination of MDMA with other drugs and/or alcohol also play a significant role. Therefore, laboratory analysis remains essential for comprehensive safety assessment.
Long-Term Stability of Ethyl Glucuronide in Hair: A 10-Year Retrospective Analysis of 909 Samples by LC-MS/MS.
Casati S, Ravelli A, Bergamaschi RF … +4 more , Del Fabbro M, Binelli G, Roda G, Orioli M
Drug Test Anal · 2025 Nov · PMID 40695461 · Full text
Monitoring long-term alcohol consumption is critical in forensic and public health contexts. Hair analysis of ethyl glucuronide (EtG), a direct metabolite of ethanol, has become a standard method for detecting chronic al...
Monitoring long-term alcohol consumption is critical in forensic and public health contexts. Hair analysis of ethyl glucuronide (EtG), a direct metabolite of ethanol, has become a standard method for detecting chronic alcohol use. While the reliability of EtG hair testing is well established for short- and medium-term analyses, its stability in hair stored over extended periods has not been comprehensively evaluated. This limitation is especially relevant in retrospective investigations, postmortem evaluations, and long-term epidemiological studies, where archived samples may be analyzed years after collection. In this study, we assessed the long-term stability of EtG in human hair stored for up to 10 years. A total of 909 samples originally analyzed between 2013 and 2022 were re-tested in 2023 using a previously published and validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. When the results of the old and the new analyses were compared, EtG concentrations showed no significant degradation over time, with more than 80% of the samples displaying matching values when analytical uncertainty was considered. Only a small fraction of samples (4.4%) dropped below the commonly used interpretive threshold for chronic alcohol use (30 pg/mg) after 10 years of storage. These findings provide robust evidence that EtG remains chemically stable in hair under standard storage conditions over a decade, confirming the reliability of archived samples for assessing alcohol use history and expanding the utility of EtG analysis in long-term toxicological and forensic investigations. The demonstrated stability strengthens confidence in hair as a matrix for retrospective substance use evaluation across scientific disciplines.
Detection of a Single Microdose of Testosterone and Recombinant EPO in Healthy Volunteers.
Heiland C, Hopcraft O, Johanson M … +3 more , Pohanka A, Lehtihet M, Ekström L
Drug Test Anal · 2025 Nov · PMID 40690983 · Full text
Doping with testosterone (T) and erythropoietin (EPO) in low doses (micro-doping) is a challenge to detect. Here, we have investigated the ability to detect micro-doping of recombinant human (rhEPO) and testosterone (T)...
Doping with testosterone (T) and erythropoietin (EPO) in low doses (micro-doping) is a challenge to detect. Here, we have investigated the ability to detect micro-doping of recombinant human (rhEPO) and testosterone (T) after administration of a single dose of subcutaneous Eporatio (15 IU/kg) and transdermal Testogel (100 mg) to healthy males. For rhEPO detection in urine, MAIIA EPO purification kits 3F6 (#1410) and 7D3 (#1460) were used for ITP and CP analyses, respectively, whereas kit 3F6 (#1430) was used for dried blood spots (Tasso). The sensitivity to detect rhEPO in Tasso was investigated and compared with previous detection results for Capitainer and Mitra. For T detection, the urinary and capillary serum steroid profile and IRMS analysis were performed. It was possible to detect administration of 15 IU/kg Eporatio with high sensitivity with our ITP method up to 72 h after administration, and the CP findings supported the ITP findings. Tasso provides less sensitivity in detecting Eporatio than Mitra and Capitainer. With IRMS, 100% of the samples analyzed were positive, also when not associated with elevated urinary T/E or 5αAdiol/E ratios. As an alternative, high systemic T levels aligned with positive IRMS results, highlighting the value of serum T as a complementary biomarker. Overall, the World Anti-Doping Agency ITP and CP methods employed today show good sensitivity towards detection of micro-dosing of rhEPO and T.
Method Development of Pegmolesatide for Doping Analysis: A Novel Synthetic Erythropoietin-Mimetic Agent.
Liu L, Wang Z, Zhao L … +2 more , Zhou X, Zhang L
Drug Test Anal · 2025 Nov · PMID 40675650 · Publisher ↗
Pegmolesatide, a novel synthetic erythropoietin-mimetic agent, was developed by the Hansoh Pharmaceutical Manufacturing Company Ltd. (Jiangsu, China). In late 2023, it was approved in China for the treatment of anemia in...
Pegmolesatide, a novel synthetic erythropoietin-mimetic agent, was developed by the Hansoh Pharmaceutical Manufacturing Company Ltd. (Jiangsu, China). In late 2023, it was approved in China for the treatment of anemia in both dialysis and non-dialysis patients with chronic kidney disease, with the advantages of reduced immunogenicity and extended duration of action. The aim of this study was to develop a strategy for detecting pegmolesatide in doping analysis. Here, we present a bottom-up nano-liquid chromatography-high-resolution tandem mass spectrometry approach for qualitative analysis of pegmolesatide using erythropoietin receptor coupled magnetic beads, followed by trypsinization and subsequent detection of characteristic peptides. Using full scan and data-dependent MS/MS (ddMS2) modes, two characteristic peptide segments of pegmolesatide were identified. An analytical method using product ion scan mode was developed to detect the identified characteristic peptides. Both peptide segments were analyzed for the initial testing procedure, whereas one characteristic peptide segment obtained from complete trypsinization was analyzed for the confirmation procedure. After full validation, the selectivity, reliability, limit of detection, limit of identification, carryover, and stability were evaluated. The results demonstrate that our developed method can be a fit-for-purpose analytical method for the antidoping of pegmolesatide.
Comprehensive Screening of Multiple Prohibited Substances in Chinese Traditional Patent Medicine by UHPLC-Q-Orbitrap HRMS.
Fei Q, Feng Y, Wang J … +8 more , Li J, Zhang H, Jing J, Wu X, Lu J, Ma Y, Xu Y, Wang X
Drug Test Anal · 2025 Nov · PMID 40664471 · Publisher ↗
An ultrahigh performance liquid chromatography coupled with quadrupole-Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) system was established for the rapid screening of doping agents in Chinese traditi...
An ultrahigh performance liquid chromatography coupled with quadrupole-Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) system was established for the rapid screening of doping agents in Chinese traditional patent medicine (CTPM), aiming to enhance the prevention and control of doping risks associated with herbal medicines. Samples were extracted by ultrasonic extraction with acetonitrile, while oily CTPM samples were extracted with 80% acetonitrile in water and purified using a Captiva EMR General Pigmented Dry cartridge. The extraction was concentrated under nitrogen flow, and the residues were dissolved, filtered, and detected using a Thermo Scientific UHPLC-Q-Orbitrap HRMS system. Separation was performed on an Agilent Zorbax Eclipse C18 column at 40°C with an injection volume of 5 μL and a gradient elution of 10-mM ammonium formate solution (pH 3.6) and acetonitrile as the mobile phase. The subsequent analysis was conducted using dual electrospray ionization in the Full MS/data-dependent secondary mass spectrometry scan mode. The method covers a total of 303 substances from 12 categories. Over 95% of the targets had limits of detection at or below 50 ng·g or ng·mL in CTPM. The method was validated for qualitative identification, including assessments of specificity, sensitivity, robustness, extraction recovery, matrix effect, and precision. The applicability of the method was demonstrated by the successful detection of higenamine (54%), ephedrine (42%), strychnine (11%), and morphine (2%) in 100 authentic samples. This paper presents a method for the rapid screening of doping agents in CTPM with high resolution, accuracy, and retrospectivity, reducing the risks of herbal medicine-induced doping violations.
Avoid Falsely Accusing Female Athletes Who Use Levonorgestrel of Doping.
Andersson A, Pohanka A, Lehtihet M … +1 more , Ekström L
Drug Test Anal · 2025 Nov · PMID 40639832 · Full text
Athletes are explicitly responsible for everything they consume, which may be an issue when the metabolic pathways of prohibited and non-prohibited compounds intersect. This was the case when 18-methyl-19-noretiocholanol...
Athletes are explicitly responsible for everything they consume, which may be an issue when the metabolic pathways of prohibited and non-prohibited compounds intersect. This was the case when 18-methyl-19-noretiocholanolone, an 18-methyl-19-nortestosterone metabolite, was detected in a sample of an athlete that had used an emergency contraceptive pill containing levonorgestrel. Six women were recruited to this study to elucidate the link between 18-methyl-19-noretiocholanolone and levonorgestrel. After providing a pre-treatment urine sample, one tablet of NorLevo, 1.5 mg, was ingested and six additional urine samples were collected. The samples were analysed with GC-MS/MS after extraction and derivatisation. In all six participants, 18-methyl-19-noretiocholanolone could be detected at 1.5-2.5 ng/mL with a t of 2 h. The presence of 18-methyl-19-noretiocholanolone was in all samples accompanied by levonorgestrel and its metabolite tetrahydronorgestrel, the latter being present at highest concentrations (60-300 ng/mL) up to 48 h post intake. Conclusively, this study demonstrates a metabolic link between 18-methyl-19-noretiocholanolone and levonorgestrel, confirming the need to verify the absence of levonorgestrel or its markers before reporting an adverse analytical finding.
"Do It Yourself" Synthetic Cannabinoid Receptor Agonist Precursors as a Ban-Evading Strategy: Comparison of the Pharmacological Characteristics of Precursors and Their Final Products.
Deventer MH, Krotulski AJ, Stove CP
Drug Test Anal · 2025 Nov · PMID 40629955 · Publisher ↗
The enactment of the generic ban on synthetic cannabinoid receptor agonists (SCRAs) in China (2021) added a new flavor to the already diverse and complex SCRA market. Although a large portion of SCRAs is covered by this...
The enactment of the generic ban on synthetic cannabinoid receptor agonists (SCRAs) in China (2021) added a new flavor to the already diverse and complex SCRA market. Although a large portion of SCRAs is covered by this legislation, a novel strategy to bypass the ban has emerged. So-called "DIY" (do-it-yourself) kits and semi-finished SCRAs are now being offered online, allowing users or intermediate suppliers to purchase ban-evading precursors, with the aim that buyers finish the synthesis. Using in vitro β-arrestin2 recruitment bioassays, we assessed the CB and CB receptor activation potential of three methyl-3,3-dimethyl-butanoate SCRA precursors (MDMB-ICA, MDMB-INACA, and MDMB-5'Me-INACA), along with some of their potential finished end products, including typical, well-known but scheduled SCRAs (e.g., 5F-MDMB-PINACA and 5F-MDMB-PICA), as well as some more recent substances (MDMB-BUTICA). Whereas tail-less precursors were weakly active at CB (EC values of 2.34 μM and higher), "finished" SCRAs ((4F-)MDMB-BUTI (NA)CA and (5F-)MDMB-PI (NA)CA) strongly activated CB (EC 1.01-35 nM and E 366%-488% [relative to JWH-018]). This emphasizes that this "DIY" synthesis phenomenon poses a serious threat to public health, as it is a new indirect way of "legally" providing users with very potent (known) compounds. Importantly, the "DIY" strategy currently ensures the continued presence of scheduled substances on the market, as exemplified by forensic cases from the United States. While precursors can often not be detected because of a concentration below the limit of detection, it is hypothesized that the presence of SCRAs in at least some of these cases stems from this ban-evading strategy.
Determining the Compliance of the Sysmex XR-1000 Haematology Analyser With WADA Athlete Biological Passport Specifications.
Voss SC, Schwenke D, Hempel J … +4 more , Mirtschink P, Wevelsiep A, Gaborini L, Robinson N
Drug Test Anal · 2025 Nov · PMID 40628496 · Publisher ↗
The athlete biological passport (ABP) has been established as an anti-doping tool based on the statistical analyses of an athlete's biological variables over a period of time. It was introduced in 2007. An important aspe...
The athlete biological passport (ABP) has been established as an anti-doping tool based on the statistical analyses of an athlete's biological variables over a period of time. It was introduced in 2007. An important aspect to ensure interlaboratory comparability was to use only one analytical platform-the Sysmex XT-2000. When the new Sysmex XN-1000 platform replaced the XT-2000i in 2019, there was a bias for the reticulocyte percentage. Although clinically insignificant, it interfered with interpreting athletes' haematological profiles for anti-doping purposes; therefore, it was necessary to adjust the haematological module. With the introduction of the new Sysmex XR-Series in 2023, an implementation of this new instrument could become necessary in the future. While the analytical performance of the XR-Series for clinical purposes has been evaluated previously, data in the context of ABP requirements, which are defined in WADA's technical documents, are not available. Therefore, our goals were to compare the XR-series with the XN-1000 and to evaluate their performance within an anti-doping context. Over 300 samples were analysed on the two instruments following WADA's technical document TD2021BAR, which defines the analytical requirements. The results for all ABP parameters including the calculated OFF-Score (OFF-hr) and the Abnormal Blood Profile Score (APBS) showed excellent interplatform comparability. In conclusion, our study demonstrates that the Sysmex XR meets WADA's requirements for haematological analysis. It can confidently replace the Sysmex XN in anti-doping laboratories without compromising the integrity of WADA's ABP longitudinal profiles.
Structural Characterization of Nitazene Analogs Using Electrospray Ionization-Tandem Mass Spectrometry (ESI-MS/MS).
Hardwick EK, Davidson JT
Drug Test Anal · 2025 Nov · PMID 40611807 · Publisher ↗
Nitazene analogs are potent novel synthetic opioids (NSOs) that are becoming increasingly common and pose a threat to the public because of their fentanyl-like effects. Although 12 nitazene analogs are currently classifi...
Nitazene analogs are potent novel synthetic opioids (NSOs) that are becoming increasingly common and pose a threat to the public because of their fentanyl-like effects. Although 12 nitazene analogs are currently classified as Schedule I under the U.S. Controlled Substances Act, novel analogs continue to emerge, making their identification in forensic laboratories exceedingly difficult. Liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) is commonly utilized in toxicology laboratories and is becoming more common for seized drug analysis, particularly for compounds less suited for gas chromatography-electron ionization-mass spectrometry (GC-EI-MS). This study provides a comprehensive structural characterization of 38 representative nitazene analogs using LC-ESI-MS/MS instrumentation, including the proposed fragmentation mechanisms that lead to the formation of diagnostic product ions, enabling analog differentiation. General fragmentation pathways and mechanisms are proposed for all nitazene analogs, including inductive cleavages and molecular rearrangements. Overall, the most common product ions for nitazene analogs are derived from the substitutions to the amine or benzyl moieties, such as m/z 100, m/z 72, m/z 44, and m/z 107. However, the presence of different substitutions shifts the observed product ions. For example, recently occurring piperidine or pyrrolidine rings produce diagnostic product ions at m/z 112 and m/z 98, respectively. Therefore, modification to the core nitazene structure produces different diagnostic product ions, which can be used to identify existing and novel analogs. This study provides a comprehensive assessment of the fragmentation behavior of nitazene analogs under ESI-MS/MS conditions, which provides the basis for identifying new structural modifications in novel nitazene analogs.
Self-Reported Use of Thyroid Hormones by Athletes at the Olympic Games.
Stuart M, Rhumorbarbe D, Kinahan A … +3 more , Gild ML, Clifton-Bligh R, Handelsman D
Drug Test Anal · 2025 Nov · PMID 40605400 · Publisher ↗
Thyroid hormones (TH) are widely used for treatment of hypothyroidism or thyroid cancer in medical practice, but their use among elite athletes without thyroid disease remains controversial. Despite lacking clear ergogen...
Thyroid hormones (TH) are widely used for treatment of hypothyroidism or thyroid cancer in medical practice, but their use among elite athletes without thyroid disease remains controversial. Despite lacking clear ergogenic benefits, some athletes reportedly use thyroxine (T4) and/or triiodothyronine (T3) with the belief that they enhance performance or facilitate weight management. This study investigates self-reported TH use by athletes at the Tokyo 2020, Beijing 2022, and Paris 2024 Olympic Games, analyzing trends based on sex, age, country, and sport. Across these three events, 1.7% of tested athletes reported TH use, with reported use higher among females and in explosive power sports, which is higher than expected for the youthful Olympic participants studied. However, TH use has declined to 1.3% at Paris 2024 compared to the previous Games (Tokyo 2020: 1.8%; Beijing 2022: 2.7%). Whether this decline is due to a growing awareness of the potential harms and/or lack of performance benefits could not be determined by this study.
Metabolic Studies of Nandrolone Decanoate in Castrated Horses After Intramuscular Administration.
So YM, Kwok WH, Tang CWY … +3 more , Wong COL, Wan TSM, Ho ENM
Drug Test Anal · 2025 Nov · PMID 40589378 · Publisher ↗
This paper describes the studies of the in vitro biotransformation of nandrolone decanoate and its metabolic fate in equine plasma and urine after intramuscular administration to castrated thoroughbred horses. The in vit...
This paper describes the studies of the in vitro biotransformation of nandrolone decanoate and its metabolic fate in equine plasma and urine after intramuscular administration to castrated thoroughbred horses. The in vitro metabolic study was performed using homogenised horse liver, and the more prominent in vitro biotransformation pathways were found to include hydrolysis, reduction, oxidation and sulfation, mainly resulting in seven Phase I metabolites and one Phase II metabolite. The administration study of nandrolone decanoate was carried out using three retired thoroughbred geldings, each of which was administered intramuscularly with 800 mg of nandrolone decanoate (Deca-Durabolin) once weekly for three consecutive weeks. Nandrolone decanoate and the majority of the identified in vitro metabolites were detectable in post-administration plasma samples for at least 20 days (last sample collected) after the last administration. Although nandrolone decanoate was not found in any post-administration urine, nandrolone (as a metabolite) and its downstream metabolites can be detected for at least 20 days post-administration (last sample collected). For doping control purpose, nandrolone decanoate itself could be a suitable target analyte in horse plasma for effectively controlling its misuse in equine sports.
Toward a Cannabis Terroir: Untargeted Metabolomic Profiling of Authentic Samples Using Gas Chromatography-High-Resolution Mass Spectrometry (GC-HRMS) and Liquid Chromatography-High-Resolution Tandem Mass Spectrometry (LC-HRMS/MS).
Poetzsch SN, Poetzsch M, Kraemer T … +1 more , Steuer AE
Drug Test Anal · 2025 Oct · PMID 40589191 · Full text
Cannabis sativa L. constituents, such as cannabinoids, terpenes, flavonoids, and other secondary metabolites, determine the plant's (medicinal) effects and properties in a complex interplay, a phenomenon known as the ent...
Cannabis sativa L. constituents, such as cannabinoids, terpenes, flavonoids, and other secondary metabolites, determine the plant's (medicinal) effects and properties in a complex interplay, a phenomenon known as the entourage effect. However, environmental influences like cultivation method, soil, light, and climate might also influence the plant's chemical composition-and thus its therapeutic profile. Much like in viticulture, the concept of a "cannabis terroir" might play an important role in determining the plant's chemical phenotype. The aim of this study was therefore to make these complex properties analytically accessible and develop a comprehensive metabolomics workflow using gas chromatography-high-resolution mass spectrometry (GC-HRMS) and liquid chromatography-high-resolution tandem mass spectrometry (LC-HRMS/MS) in positive and negative ionization mode, applying HILIC and reversed phase chromatography to assess multiple chemical classes. Data processing and statistical analysis were done in MS-DIAL and MetaboAnalyst, respectively. The method was applied to 35 CBD-type cannabis flowers grown under different environmental conditions, and compounds belonging to various chemical classes were successfully detected. Principal component analysis revealed distinct clustering of the samples, and key discriminative features were identified, including cannabinoids, terpenes such as β-caryophyllene and α-humulene, cuticular alkanes (e.g., pentacosane and nonacosane), and polar compounds such as choline and trigonelline. The markers enabled a discrimination of samples not only by chemical phenotype but also by cultivation environment, supporting the emerging concept of a cannabis terroir. In conclusion, this study introduces an analytical framework for the comprehensive chemical profiling of cannabis employing GC-HRMS and LC-HRMS analysis and advanced statistical techniques.
SARMs, Metabolic Modulators and Growth Hormone Secretagogues in Suspected Illegal Medicines, Bought as Sport Performance Enhancers: A Retro- and Prospective Study Within the GEON.
Barrios MM, Deconinck E, Vanhee C … +24 more , Lamme EK, 't Hart-Bakker I, Syversen PV, Bøyum O, Li-Ship G, Young S, Blazewicz A, Poplawska M, Hakkarainen B, Huynh NH, Hackl A, Portela MJ, Martinho P, Beerbaum N, Gaudiano MC, Raimondo M, Marleau V, Cloutier J, Ollerenshaw J, Hansen A, Mills J, Aha M, Luchte C, Miquel M
Drug Test Anal · 2025 Oct · PMID 40551438 · Publisher ↗
Although the abuse of muscle-building compounds in elite sports is already known for a long time, these products have become more popular in recreational sport over the past years. Although anabolic steroids are still th...
Although the abuse of muscle-building compounds in elite sports is already known for a long time, these products have become more popular in recreational sport over the past years. Although anabolic steroids are still the most popular ones in this context, the use of other molecules with anabolic properties is on the rise. Three categories of such products are the selective androgen receptor modulators (SARMs), the metabolic modulators and the growth hormone secretagogues (GHS). Based on this trend and the outcomes of a previous market surveillance study in the domain of illegal products (MSSIP), the Falsified Medicines Working Group of the General European Official Medicines Control Laboratories (OMCL) Network (GEON) decided to conduct an MSSIP with focus on SARMs, metabolic modulators and GHS over a period of 5 years. In total 324 samples and 354 results, reported by 14 laboratories in 13 countries, members of the GEON, were taken into account, for which the majority of the samples originated from illegal distribution. Sixty-five percent of the seized products were represented as medicine, though 24% as dietary supplements, which is of concern because here the (recreational) sporter is not aware he is taking an (unapproved) pharmaceutical. Eighteen different molecules, within the scope of the study, were reported with as top 5: ibutamoren, ligandrol, ostarine, cardarine and andarine. From the limited quantitative data reported, it can be assumed that the majority of the samples contain active doses and some are even overdosed, so health risks for the consumers cannot be neglected.
Development of an Optimized Extraction Method to Recover Drug Material From Used Test Strips for Comprehensive Drug Checking.
Appley MG, Pyfrom EM, Elkasabany RA … +2 more , Rousch R, Sisco E
Drug Test Anal · 2025 Oct · PMID 40532942 · Publisher ↗
Drug-checking programs use point-of-need testing (e.g., test strips) and laboratory-based analysis to rapidly identify emerging drug threats, but each has limitations. Test strips are quick but compound or class specific...
Drug-checking programs use point-of-need testing (e.g., test strips) and laboratory-based analysis to rapidly identify emerging drug threats, but each has limitations. Test strips are quick but compound or class specific, whereas laboratory testing can identify more compounds but have lengthy turnaround times. To address these limitations, it was proposed that compounds could be extracted from used test strips for additional analyses allowing for rapid on-site information followed by comprehensive laboratory results. The method development process involved four parts: determining the optimal extraction approach, assessing the feasibility of performing direct analysis in real-time mass spectrometry (DART-MS) analysis on extracts, determining the limits of detection (LODs) for a range of analytes, and evaluating the method using used test strips submitted by harm reduction sites. The optimized method consisted of extracting analytes of interest from a cut test strip using 0.5-mL methanol while vortexing for 10 s. DART-MS successfully identified the compounds of interests, and the test strip chemical background was identified. LODs were found to be as low as a mass fraction of 0.005 in a mixture. For the samples submitted by harm reduction sites, concordance between extracts and test strip results was 96%, and the agreement in compound identification between used test strip extracts and authentic drug collection samples was approximately 80% regardless of test strip type and preparation. This work shows that additional analyses of extracted test strips can provide a low-barrier way for high-quality testing that can be used to increase data on the drug landscape.
Monitoring Community Use of Benzodiazepines Through Wastewater-Based Epidemiology.
Quireyns M, Boogaerts T, Van Wichelen N … +9 more , Vanaga-Arāja D, Rudminienė O, Iliescu R, Georgescu M, Schaerlaekens S, De Roeck N, Delputte P, Covaci A, van Nuijs ALN
Drug Test Anal · 2025 Oct · PMID 40532898 · Publisher ↗
Benzodiazepines and related z-drugs (BZDs) are widely used pharmaceuticals but require careful monitoring due to limited efficacy, tolerance development and the risk of dependence. Wastewater-based epidemiology (WBE) is...
Benzodiazepines and related z-drugs (BZDs) are widely used pharmaceuticals but require careful monitoring due to limited efficacy, tolerance development and the risk of dependence. Wastewater-based epidemiology (WBE) is a valuable approach to gather population-wide information on consumption patterns through analysis of influent wastewater. This study examines how overlapping metabolic pathways within the BZD drug class can lead to misinterpretation if not carefully considered. An analytical method is developed and validated for 26 biomarkers of prescription BZDs in influent wastewater using solid-phase extraction and liquid chromatography-tandem mass spectrometry and applied to influent wastewater samples for the first time in Belgium (13 locations), Latvia (1), Lithuania (3) and Romania (1). The countries were chosen for their differing prescription BZD market registration, allowing testing of different hypotheses. To aid in complex data interpretation, this study presents a structured categorisation of BZDs into direct biomarkers, which directly reflect consumption, and downstream biomarkers, which are influenced by multiple BZDs, and further discusses the implication this has on the interpretation. Spatial differences were noted among direct biomarkers such as higher consumption of zolpidem in Belgium and zopiclone in Riga (LVA). Downstream biomarkers had higher population-normalised mass loads but cannot be interpreted in isolation, for example, lorazepam (ranging 4-25 mg/day/1000 inhabitants over all locations), lormetazepam (8-30), oxazepam (10-50) and temazepam (1-12). These findings highlight challenges in interpreting BZD consumption trends and emphasise the need of distinguishing different biomarker classes to ensure accurate and comparable results across studies needed to guide informed decision-making.
Analysis of Methyltestosterone and Testosterone Propionate in Dried Blood Spots After Transdermal Application.
Miyamoto A, Okano M, Ota M … +1 more , Sato M
Drug Test Anal · 2025 Oct · PMID 40474335 · Publisher ↗
In the past few years, doping tests have been performed with dried blood spots (DBS) as test samples; this sampling method is minimally invasive and requires minimal storage space. Steroid esters are stable in dried bloo...
In the past few years, doping tests have been performed with dried blood spots (DBS) as test samples; this sampling method is minimally invasive and requires minimal storage space. Steroid esters are stable in dried blood, allowing the direct analysis of testosterone esters. In Japan, the cream-based formulation containing 17α-methyltestosterone (MeT) and testosterone propionate (TP) is available as an over-the-counter drug for hair growth. Here, we investigated whether the transdermal uptake of this formulation could be detected using the existing method for steroid ester analysis in DBS. A method that was previously validated to detect and identify TP could also detect MeT. We developed a high throughput liquid chromatography-tandem mass spectrometry method to identify MeT in DBS. The limits of detection and identification of MeT were 0.1 ng/mL and 0.6 ng/mL, respectively. Five male human subjects received the cream-based formulation of MeT and TP transdermally. We then collected blood samples by finger pricking and made DBS on cellulose paper. Using this method, MeT was detected and identified up to 97 h after the final application. TP was also detected up to 97 h and identified up to 49 h after the final application. The developed method provides a direct confirmation of the presence of the drug. Moreover, using cream preparations could lead to contamination from MeT and TP remaining on the fingertip skin during fingertip puncture sampling.
Detection of Transdermal Application of Testosterone to Racehorses by Analysis of Urine and Plasma.
Viljanto M, Cutler C, Habershon-Butcher J … +2 more , Hincks P, Scarth J
Drug Test Anal · 2025 Oct · PMID 40461131 · Publisher ↗
The use of testosterone in racehorses is predominantly monitored using international urine and plasma concentration-based thresholds and complementary steroid ratios. To date, there has been no published pharmacokinetic...
The use of testosterone in racehorses is predominantly monitored using international urine and plasma concentration-based thresholds and complementary steroid ratios. To date, there has been no published pharmacokinetic study on transdermally applied testosterone products in horses and whether their use could result in adverse analytical findings. Therefore, quantitative analysis of testosterone and epitestosterone in urine and testosterone in plasma samples was performed following a pilot multi-dose transdermal Testogel administration (1 mg/kg once a day for 7 days on clipped skin) to one gelding and one mare. The peak concentrations (C) of free testosterone were 1060 and 1800 pg/mL in gelding and mare plasma, respectively. Testosterone concentrations exceeded the international plasma threshold of 100 pg/mL consistently for up to 4 h post-administration, after which detection above the threshold was sporadic up to 127 h. In urine, C of free and conjugated (sulfate and glucuronide) testosterone were 700 and 323 ng/mL in gelding and mare urine, respectively. In the gelding, testosterone concentrations exceeded the international urine threshold of 20 ng/mL consistently for up to 47 h post-administration, but sporadically up to 143 h. In all samples, testosterone: epitestosterone ratios were greater than 5, another requirement for adverse analytical findings in geldings. In the mare, testosterone concentrations exceeded the urine threshold of 55 ng/mL consistently for up to 71 h post-administration, but sporadically up to 167 h. Therefore, these limited results for one gelding and one mare demonstrate that doping control following transdermal applications of testosterone to racehorses is possible using existing approaches.
A "Pheraplex" Capsule Labeled as Desoxymethyltestosterone From the Market Turned Out to Be 17,17-Dimethyl-18-nor-5α-androst-13-en-3β-ol.
Zhu S, Wang S, Liu X … +1 more , Zhang L
Drug Test Anal · 2025 Oct · PMID 40405720 · Publisher ↗
In an effort to conduct a desoxymethyltestosterone (DMT) administration study to replenish excretion urine inventory of Beijing Anti-Doping Laboratory for quality assurance purpose, a product labeled as "Pheraplex" was p...
In an effort to conduct a desoxymethyltestosterone (DMT) administration study to replenish excretion urine inventory of Beijing Anti-Doping Laboratory for quality assurance purpose, a product labeled as "Pheraplex" was purchased from the internet. The product's label indicated that each capsule contained 10 mg of 17α-methyl-etioallocholan-2-ene-17β-ol (DMT), along with medicinal corn starch and gelatin. To verify the product's contents, gas chromatography tandem quadrupole mass spectrometry (GC-MS/MS) was employed to analyze the active ingredient and compare it with the reference materials of DMT. Surprisingly, the results revealed that the product did not contain DMT or any other steroids monitored in the initial testing procedure of our laboratory. Subsequently, nuclear magnetic resonance was utilized to identify the compound's structure, which was determined to be 17,17-dimethyl-18-nor-5α-androst-13-en-3β-ol. This compound was referred to as M10 of 17α-methyltestosterone in a literature. This finding highlights the potential discrepancies between product labeling and actual contents in the supplement market, which deserves attention from the anti-doping community.
Evaluation of Diagnostic Sensitivity and Specificity of a New Automatized Assay for Indirect Synthetic Urine Identification.
Franke L, Fuczik C, Wissenbach DK
Drug Test Anal · 2025 Oct · PMID 40405346 · Publisher ↗
Synthetic urine mimicking normal urine is difficult detectable by standard specimen validity testing. In this study, the VDx True Urine LD Test and True Urine SD Test, analysing 'long duration' (LD) and 'short duration'...
Synthetic urine mimicking normal urine is difficult detectable by standard specimen validity testing. In this study, the VDx True Urine LD Test and True Urine SD Test, analysing 'long duration' (LD) and 'short duration' (SD) markers, were evaluated for their ability to detect synthetic urine. Two synthetic urines from the US market and 1188 real-life urine specimens were analysed for LD markers, SD markers, uric acid and temperature. Forty-seven specimens (set 1) showed uric acid and/or temperature suspicious results and were analysed by LC-MS/MS for 10 endogenous biomolecules. Diagnostic sensitivities and specificities were calculated for LD and SD markers based on uric acid and LC-MS/MS results of set 1. The false-positive rate of the SD marker was further evaluated with uric acid results of the other 1141 specimens (set 2). Additionally, direct synthetic urine markers were analysed by LC-(HR)MS. Uric acid and LC-MS/MS could identify synthetic urine. In one US synthetic urine, low concentrations of uric acid were found. Specimens of the Austrian/German region were reliably classified congruently by both methods. The LD and the SD markers detected both synthetic urines. For set 1, the LD had 100% sensitivity and 88.9% specificity, and the SD had 84.2% sensitivity and 44.4% specificity for authentic/synthetic specimens. In set 2, the SD marker specificity depended on the upper limit of the acceptance criteria. In one US synthetic urine, carbendazim was identified. Overall, several tests should be applied to confirm authentic or synthetic urine. Especially, simultaneous analysis of indirect and direct synthetic urine markers should be considered.
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