Drug Testing and Analysis最新文献

{"title":"Comprehensive Screening of Multiple Prohibited Substances in Chinese Traditional Patent Medicine by UHPLC-Q-Orbitrap HRMS.","authors":"Qiaoling Fei, Yiman Feng, Jiarui Wang, Jing Li, Huiwu Zhang, Jing Jing, Xiaopei Wu, Jianghai Lu, Yanhua Ma, Youxuan Xu, Xiaobing Wang","doi":"10.1002/dta.3929","DOIUrl":"https://doi.org/10.1002/dta.3929","url":null,"abstract":"<p><p>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^-1 or ng·mL^-1 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.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144641333","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Identification of Novel THC Analogs: Chloro Derivatives of Hexahydrocannabinol and Tetrahydrocannabibutol Butanoate in an Oil Product Obtained in Japan.","authors":"Rie Tanaka, Maiko Kawamura, Michiho Ito, Ruri Kikura-Hanajiri","doi":"10.1002/dta.3927","DOIUrl":"https://doi.org/10.1002/dta.3927","url":null,"abstract":"<p><p>Since around 2021, products such as e-cigarette liquid cartridges, herbal products, and gummy products, claiming to contain tetrahydrocannabinol (THC) analogues, have been seen for sale on the internet. Recently, products claiming to contain other THC derivatives have appeared. In this study, we identified the ingredients in products distributed on the internet that claim to contain THC derivatives. The e-cigarette cartridge product analyzed in this study was obtained from Japan in September 2024. One milligram of the oil product was treated with 1 mL of acetonitrile under ultrasonication. The resulting solutions were used for gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-photodiode array-mass spectrometry (LC-PDA-MS) measurements. After isolating and purifying unknown components from the product, structural analysis was performed by measuring ¹H, ¹³C nuclear magnetic resonance (NMR) and various two-dimensional NMR (COSY, HMQC, HMBC, and NOESY) and LC with hybrid quadrupole time-of-flight MS. The analysis revealed that chlorinated HHCs (i.e., (9R)-2-chloro-HHC, (9S)-2-chloro-HHC, (9R)-4-chloro-HHC, (9S)-4-chloro-HHC, (9R)-2,4-dichloro-HHC, and (9S)-2,4-dichloro-HHC) were the major components, and chlorinated dihydro-iso-THCs (i.e., 10-chloro-dihydro-iso-THC, 8-chloro-dihydro-iso-THC, and 8,10-dichloro-iso-THC) were the minor components isolated and identified from the product. Furthermore, Δ⁹-THCB-O-butanoate, a compound in which the hydroxyl group at the C1 position of Δ⁹THCB was butanoylated, was detected.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144937305","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Post-Mortem Identification and Toxicological Findings of Fluetonitazepyne and Isotonitazepyne.","authors":"Pirkko Kriikku, Anna Pelander, Antti Jylhä, Ilkka Ojanperä","doi":"10.1002/dta.3928","DOIUrl":"https://doi.org/10.1002/dta.3928","url":null,"abstract":"<p><p>Nitazepyne-type substances, such as fluetonitazepyne and isotonitazepyne, are among the latest additions to the group of nitazenes-highly potent and dangerous opioids that have emerged on the illicit drug market in recent years. In early 2025, five death cases in Finland tested positive for fluetonitazepyne and one for isotonitazepyne in urine drug screening. The median (range) concentration of fluetonitazepyne in post-mortem femoral blood was 1.7 (0.4-9.5) μg/L, and the concentration of isotonitazepyne was 1.4 μg/L. Other psychoactive substances were detected in all cases. A peak corresponding to O-dealkylated fluetonitazepyne, the 4-OH-nitazepyne metabolite, was present in all fluetonitazepyne-positive urine samples and was later used in the identification of isotonitazepyne in one fatal case. This metabolite proved useful as a marker compound for nitazepyne-type benzimidazole opioids in a urine screening.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144937348","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Avoid Falsely Accusing Female Athletes Who Use Levonorgestrel of Doping.","authors":"Alexander Andersson, Anton Pohanka, Mikael Lehtihet, Lena Ekström","doi":"10.1002/dta.3925","DOIUrl":"https://doi.org/10.1002/dta.3925","url":null,"abstract":"<p><p>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_max 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.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606944","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"\"Do It Yourself\" Synthetic Cannabinoid Receptor Agonist Precursors as a Ban-Evading Strategy: Comparison of the Pharmacological Characteristics of Precursors and Their Final Products.","authors":"Marie H Deventer, Alex J Krotulski, Christophe P Stove","doi":"10.1002/dta.3924","DOIUrl":"https://doi.org/10.1002/dta.3924","url":null,"abstract":"<p><p>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 CB₁ and CB₂ 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 CB₁ (EC₅₀ values of 2.34 μM and higher), \"finished\" SCRAs ((4F-)MDMB-BUTI (NA)CA and (5F-)MDMB-PI (NA)CA) strongly activated CB₁ (EC₅₀ 1.01-35 nM and E_max 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.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144590023","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determining the Compliance of the Sysmex XR-1000 Haematology Analyser With WADA Athlete Biological Passport Specifications.","authors":"S C Voss, D Schwenke, J Hempel, P Mirtschink, A Wevelsiep, L Gaborini, N Robinson","doi":"10.1002/dta.3926","DOIUrl":"https://doi.org/10.1002/dta.3926","url":null,"abstract":"<p><p>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.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144590024","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Structural Characterization of Nitazene Analogs Using Electrospray Ionization-Tandem Mass Spectrometry (ESI-MS/MS).","authors":"Emma K Hardwick, J Tyler Davidson","doi":"10.1002/dta.3921","DOIUrl":"https://doi.org/10.1002/dta.3921","url":null,"abstract":"<p><p>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.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144558552","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Self-Reported Use of Thyroid Hormones by Athletes at the Olympic Games.","authors":"Mark Stuart, Damien Rhumorbarbe, Audrey Kinahan, Matti L Gild, Roderick Clifton-Bligh, David Handelsman","doi":"10.1002/dta.3923","DOIUrl":"https://doi.org/10.1002/dta.3923","url":null,"abstract":"<p><p>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.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144551519","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Metabolic Studies of Nandrolone Decanoate in Castrated Horses After Intramuscular Administration.","authors":"Yat-Ming So, Wai Him Kwok, Christina W Y Tang, Celia O L Wong, Terence S M Wan, Emmie N M Ho","doi":"10.1002/dta.3919","DOIUrl":"https://doi.org/10.1002/dta.3919","url":null,"abstract":"<p><p>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.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144525713","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"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)","authors":"Sandra N. Poetzsch,&nbsp;Michael Poetzsch,&nbsp;Thomas Kraemer,&nbsp;Andrea E. Steuer","doi":"10.1002/dta.3922","DOIUrl":"10.1002/dta.3922","url":null,"abstract":"<p><i>Cannabis sativa L</i>. 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.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"17 10","pages":"2086-2095"},"PeriodicalIF":2.7,"publicationDate":"2025-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/epdf/10.1002/dta.3922","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144525714","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}