Bahare Makvandi, Anton Pohanka, Mats Bergström, Annica Börjesson, Mikael Lehtihet, Lena Ekström, Yufang Zheng
{"title":"Detection of anabolic androgenic steroids in serum samples","authors":"Bahare Makvandi, Anton Pohanka, Mats Bergström, Annica Börjesson, Mikael Lehtihet, Lena Ekström, Yufang Zheng","doi":"10.1002/dta.3476","DOIUrl":"10.1002/dta.3476","url":null,"abstract":"<p>When testing for anabolic androgenic steroids (AAS) outside sports communities, for example, in healthcare and forensic medicine, urine is the matrix of choice. However, there are drawbacks with urinary sampling, and serum might be useful as a complementary matrix. The aim was to develop an LC–MS/MS method for serum measuring AAS frequently used outside of sport, including testosterone (T), steroid esters, and eight other synthetic AAS. The sample pretreatment included sample precipitation and evaporation. Limit of quantification for the AAS was 0.05–0.5 ng/mL, and linearity was 0.05–20 ng/mL for most of the substances. Generally, the within- and between-day CV results, matrix effect, and process efficiency were <15%. The AAS were stable for at least 6 months at −20°C. Serum samples were obtained from previous studies. A novel finding from an administration study was that T enanthate was present in serum even after 5 years of storage at −20°C. Serum samples from self-reporting AAS individuals, where T esters were detected, were positive for testosterone using the urinary testosterone/epitestosterone criterion >10. Of those identified as positive in traditional urinary doping tests (<i>n</i> = 15), AAS in serum were found in 80% of the subjects. Our results show that serum may be a valid complementary matrix to urine samples for AAS testing.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"15 6","pages":"678-688"},"PeriodicalIF":2.9,"publicationDate":"2023-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/dta.3476","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"5881514","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}
{"title":"Response to the letter to the editor “GHB-facilitated sexual assaults: How to proper assess a single GHB exposure in hair”","authors":"Serena Mestria, Sara Odoardi, Sabina Strano Rossi","doi":"10.1002/dta.3474","DOIUrl":"10.1002/dta.3474","url":null,"abstract":"","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"15 7","pages":"793-795"},"PeriodicalIF":2.9,"publicationDate":"2023-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"6072786","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}
Katja Walpurgis, Johannes Agricola, Andreas Thomas, Mario Thevis
{"title":"Myostatin inhibitory peptides in sports drug testing","authors":"Katja Walpurgis, Johannes Agricola, Andreas Thomas, Mario Thevis","doi":"10.1002/dta.3473","DOIUrl":"10.1002/dta.3473","url":null,"abstract":"<p>Across species, skeletal muscle mass is negatively regulated by the TGF-β cytokine myostatin (MSTN). Inhibitors of this growth factor and its signaling pathways are therefore not only promising therapeutics for muscular diseases but also potential performance-enhancing agents in sports. Within this study, protein precipitation and liquid chromatography high-resolution tandem mass spectrometry (LC-HRMS/MS) were employed to develop a detection method for six novel MSTN inhibitory peptides derived from the regulatory MSTN propeptide and the natural MSTN inhibitor follistatin (FST) from doping control serum samples. The approach was comprehensively characterized and found to allow for a specific detection down to concentrations of 3–9 ng/mL. Moreover, several potential metabolites of the drug candidates referred to as DF-3, DF-25, and Peptide 7 were identified as valuable complementary analytical targets for doping control analytical assays. Overall, the acquired data pave the way for an implementation of MSTN inhibitory peptides into routine sports drug testing. Even though no drug candidate has obtained clinical approval yet, a proactive development of detection assays is of utmost importance to deter athletes from misusing such compounds, which are readily available for research purposes and on the black market.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"15 11-12","pages":"1477-1487"},"PeriodicalIF":2.9,"publicationDate":"2023-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/epdf/10.1002/dta.3473","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9196242","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}
{"title":"Advances in whole aerosol approaches for in vitro e-cigarette testing","authors":"Emma Bishop, Marianna Gaça, David Thorne","doi":"10.1002/dta.3471","DOIUrl":"10.1002/dta.3471","url":null,"abstract":"<p>Electronic-cigarette regulation and risk assessment is a prominent and developing field, as the popularity and prevalence of this product category increases. Over the last 10 years since their emergence, there have been many advances and adaptations to current in vitro testing techniques to better assess and predict absolute consumer risk. However, there are still requirements to create a cross-field harmonised approach to appropriate exposure and experimental design. With many assessments still being carried out using methods developed and optimised for cigarette smoke, there must first be an acknowledgement regarding the differences between cigarette smoke and tobacco-free e-cigarette aerosols before we can accurately assess these distinct products. Here, we discuss five published studies from within our own research to demonstrate how in vitro testing techniques have evolved to improve determination of risk by considering appropriate dosimetry and exposure for both e-cigarette and cigarette aerosols and how we can contextualise the data through human consumption and dose extrapolation, ultimately giving more relevance to in vitro data. Furthermore, we have demonstrated the evolution of techniques, which has allowed us to bridge between platforms, simplify exposure set-up, experimental design and demonstrate technology evolution within our products, thus fulfilling a responsible duty of care to consumers via an appropriate and robust in vitro product assessment.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"15 10","pages":"1133-1144"},"PeriodicalIF":2.9,"publicationDate":"2023-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9223153","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}
Pia Johansson Heinsvig, Ask Vest Christiansen, Daniel Ayoubi, Laura Smedegaard Heisel, Christian Lindholst
{"title":"Do you get what you see? The illicit doping market in Denmark—An analysis of performance and image enhancing drugs seized by the police over a 1-year period","authors":"Pia Johansson Heinsvig, Ask Vest Christiansen, Daniel Ayoubi, Laura Smedegaard Heisel, Christian Lindholst","doi":"10.1002/dta.3472","DOIUrl":"10.1002/dta.3472","url":null,"abstract":"<p>This study examines doping products seized by the police in three regional police districts in Denmark from December 2019 to December 2020. The products, often referred to as performance and image-enhancing drugs (PIEDs), are described in relation to the country of origin, manufacturing company, and the active pharmaceutical ingredient (API) stated on the packaging versus the one identified by subsequent chemical analysis. The study also includes a description of the degree of professionalism by which the products appear according to EU requirements. A total of 764 products were seized during the study period. The products originate from 37 countries, mainly located in Asia (37%), Europe (23%), and North America (13%). One hundred ninety-three different manufacturing companies could be identified from the product packaging. The most frequent compound class was the androgenic anabolic steroids, found in 60% of the products. In 25%–34% of the products, either no or an incorrect API relative to the one stated on the product was found. However, only 7%–10% contain either no API or a compound from a different compound class than the one stated. Most products had a professional appearance fulfilling most EU requirements for packaging information. The study shows that many different companies supply PIEDs to the Danish market and that counterfeit and substandard products are widespread. Many products do, however, appear professional to the user giving an impression of a high-quality product. Although many products are substandard, they most often contain an API from the same compound class as the one labeled.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"15 6","pages":"668-677"},"PeriodicalIF":2.9,"publicationDate":"2023-03-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/dta.3472","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"5748492","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}
Vinod S. Nair, John D. Howa, Matthew S. Morrison, Lacey Beggs, Thane Campbell, Matthew Fedoruk, Brian Ahrens, Daniel Eichner
{"title":"δ13C values of urinary 19-norandrosterone in antidoping samples and potential for adverse findings from boar offal consumption","authors":"Vinod S. Nair, John D. Howa, Matthew S. Morrison, Lacey Beggs, Thane Campbell, Matthew Fedoruk, Brian Ahrens, Daniel Eichner","doi":"10.1002/dta.3470","DOIUrl":"10.1002/dta.3470","url":null,"abstract":"<p>19-Norandrosterone (19NA) is the preferred urinary target compound to identify doping with nandrolone or related 19-norsteroids. At concentrations between 2.5 and 15 ng/mL, isotope ratio mass spectrometry (IRMS) is required to establish exogenous origin of urinary 19NA. An absolute difference of 3‰ between urinary 19NA and an endogenous reference compound (ERC) constitutes a finding for exogenous origin of 19NA. Over the last 3 years, 77 samples containing urinary 19NA between 2.5 and 15 ng/mL were analyzed at our laboratory. The measured δ<sup>13</sup>C values for 19NA ranged from −29.5‰ to −16.8‰. In comparison, the δ<sup>13</sup>C values for the corresponding urinary ERCs ranged from −22.4‰ to −16.2‰. Due to the considerable overlap in values between the target compound and the natural range of urinary ERCs, it can be challenging to distinguish between endogenous and exogenous origins of urinary 19NA. In addition, it is well known that consumption of offal from non-castrated pigs can produce 19NA in urine. To determine whether this could cause a positive IRMS finding under the current IRMS positivity criteria, meat from non-castrated boars fed a mixture of corn and soy was consumed by 13 volunteers. Two volunteers produced 19NA findings above 2.5 ng/mL, and the measured isotope values, while inconsistent with documented 19-norsteroid preparations, did meet IRMS positivity criteria. However, these increases in 19NA urinary concentrations were short-lived due to rapid elimination. Timely follow-up collections may help support a claim for dietary exposure when low urinary concentrations of 19NA with pseudo-endogenous isotope values are observed.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"15 11-12","pages":"1356-1360"},"PeriodicalIF":2.9,"publicationDate":"2023-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9187503","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}
Tajudheen K. Karatt, M. Anwar Sathiq, Saraswathy Laya, Abdul Khader Karakka Kal, Michael Benedict Subhahar, M. P. Muhammed Ajeebsanu, Moses Philip, Marina Rodriguez Caveney, Fatma Mohammed Graiban
{"title":"In-depth metabolic study of nonsteroidal selective androgen receptor modulator GSK2881078 in thoroughbred horses and horse liver microsomes for doping control","authors":"Tajudheen K. Karatt, M. Anwar Sathiq, Saraswathy Laya, Abdul Khader Karakka Kal, Michael Benedict Subhahar, M. P. Muhammed Ajeebsanu, Moses Philip, Marina Rodriguez Caveney, Fatma Mohammed Graiban","doi":"10.1002/dta.3469","DOIUrl":"10.1002/dta.3469","url":null,"abstract":"<p>Nonsteroidal selective androgen receptor modulators (SARMs) are a novel class of compounds that have not yet been clinically approved; however, they appear to have a better anabolic/androgenic ratio than steroids and cause slighter side effects. Sports drug testing laboratories are required to maintain continuously updated doping control analytical methods in light of the widespread misuse of SARMs in elite and amateur sports. This paper describes the metabolic conversion of SARM GSK2881078 in thoroughbred horses following oral administration and in vitro with equine liver microsomes. A liquid chromatography–high-resolution mass spectrometry method was used to postulate the plausible structures of the detected metabolites. A total of five (M1–M5) in vivo metabolites and six (M1–M6) in vitro metabolites were detected under experimental conditions. Phase I metabolites mainly result from hydroxylation. Methoxylated and side-chain dissociated metabolites were also detected. Neither sulfonic acid nor glucuronic acid conjugated metabolites were observed in this study. Data reported here could aid in the detection of nonsteroidal SARM GSK2881078 and reveal its illicit use in competitive sports.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"15 7","pages":"757-768"},"PeriodicalIF":2.9,"publicationDate":"2023-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"6152837","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":"Contaminated disposable rubber gloves as evidence samples after a chemical attack with nerve agents","authors":"Tomas Rozsypal","doi":"10.1002/dta.3468","DOIUrl":"10.1002/dta.3468","url":null,"abstract":"<p>Nerve agents have been used recently in the Syrian civil war. Collecting relevant samples for retrospective identification of an attack is often problematic. The article deals with the possibility of using contaminated gloves as an analytical sample for evidence of the chemical weapons use. There have not yet been published studies dealing with the identification of chemical warfare agents in this type of matrix, where the diversity of chemical properties of gloves and the lifetime of the contaminated sample would be considered. Sarin, soman, and cyclosarin were used as contaminants in the study. Nitrile, latex, and vinyl disposable gloves were chosen as matrices. The identification method was gas chromatography. Six solvents commonly used in military laboratories were tested as extractants. The extraction procedure was optimized in terms of the appropriate method (vortex) and the required extraction time (1 min) and resulted in significant reduction in sample preparation time. The chromatographic background of the extracts was also monitored in order to find a method with the least number of peaks interfering in the identification. Suitable solvents were hexane and acetonitrile. The lifetime of the sample was also investigated. The worst result was recorded for latex. For individual contaminants, the time varied depending on the volatility. The developed procedures were successfully validated within a sample handling effects scenario. The results demonstrate that in the event of an ongoing military risk at the site of an attack, even discarded disposable rubber glove type samples can be used as evidence.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"15 7","pages":"745-756"},"PeriodicalIF":2.9,"publicationDate":"2023-03-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"5674877","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}
Christopher Russell, Willie J. McKinney, Ian M. Fearon
{"title":"Behavioral intentions assessment of a disposable e-cigarette among adult current, former, and non-smokers in the United States","authors":"Christopher Russell, Willie J. McKinney, Ian M. Fearon","doi":"10.1002/dta.3467","DOIUrl":"10.1002/dta.3467","url":null,"abstract":"<p>Modeling the public health effects of e-cigarettes requires estimates of the likelihood that different individuals and population subgroups will start using e-cigarettes and subsequently transition to and from combustible cigarette use. To begin to generate input values for modeling efforts, this study assessed adults' behavioral intentions in relation to a disposable e-cigarette, “BIDI® Stick.” An online questionnaire assessed intentions to try and use a BIDI® Stick regularly in 11 flavor variants among United States (U.S.) nationally representative samples of adult (21+ years) non-smokers (<i>n</i> = 2284), current smokers (<i>n</i> = 2391), former smokers (<i>n</i> = 2241), and young adult (21–24 years) non-smokers (<i>n</i> = 1140) of combustible cigarettes following exposure to product information and images. Current smokers rated their intentions to use a BIDI® Stick to partially or completely replace cigarettes. Positive intention to try a BIDI® Stick at least once was, for each flavor variant, highest among current smokers (22.4%–28.1%), lower among former smokers (6.0%–9.7%) and non-smokers (3.4%–5.2%), and lowest among never-smokers (1.0%–2.4%). Among current smokers, former smokers, and non-smokers, trial and regular use intentions were lowest among e-cigarette non-users and e-cigarette never-users. Approximately 23.6% of current smokers reported an intention to use a BIDI® Stick in at least one flavor to completely switch from cigarettes and/or to reduce cigarette consumption. Low trial and regular use intentions suggest that U.S. adults who do not currently smoke cigarettes and/or use e-cigarettes are unlikely to initiate use of the BIDI® Stick e-cigarette. Trial and regular use intentions are highest among adults who currently smoke cigarettes and/or use e-cigarettes. A moderate proportion of current smokers may try using a BIDI® Stick e-cigarette as a partial or complete replacement for combustible cigarettes.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"15 10","pages":"1233-1256"},"PeriodicalIF":2.9,"publicationDate":"2023-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9483651","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}
Ian M. Fearon, Ryan G. N. Seltzer, Trisha L. Houser, Andrew Tope, Xavier Cahours, Thomas Verron, Layla Malt, Thomas Nahde, Grant O'Connell, Mitchell Nides
{"title":"Curiosity and intentions to use myblu e-cigarettes and an examination of the ‘gateway’ theory: Data from cross-sectional nationally representative surveys","authors":"Ian M. Fearon, Ryan G. N. Seltzer, Trisha L. Houser, Andrew Tope, Xavier Cahours, Thomas Verron, Layla Malt, Thomas Nahde, Grant O'Connell, Mitchell Nides","doi":"10.1002/dta.3450","DOIUrl":"10.1002/dta.3450","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <p>Encouraging adult smokers who are uninterested or unwilling to quit, and would otherwise continue to smoke, to transition to potentially less harmful nicotine products such as electronic nicotine delivery systems (ENDS) may positively impact population health. However, counterbalancing this benefit is the societal concern that ENDS may be used by never smokers and youth and serve as a ‘gateway’ into cigarette smoking. Data were analysed from two independent surveys of the prevalence and perceptions of <i>my</i>blu ENDS use in the United States. Total sample size was 22,232 young adults and 23,264 adults. Being curious to use <i>my</i>blu was 1.6–2.0 times more likely in young adult current smokers than young adult never smokers. This likelihood was 2.8 times greater for adult current smokers compared with adult never smokers in the perceptions survey, while in the prevalence survey, there was no difference between adult current and never smokers. Intentions to use <i>my</i>blu were significantly greater in young adult current smokers compared with young adult never smokers in both surveys and in adults in the prevalence survey. In all surveys and age cohorts, 124 of 45,496 participants (0.1% of the total survey population) reported first using <i>my</i>blu prior to smoking cigarettes and went on to become established smokers. Curiosity and intentions to use <i>my</i>blu were generally higher in current smokers compared with never smokers. There was minimal evidence to suggest the existence of a ‘gateway’ effect to established cigarette smoking among never-smoking <i>my</i>blu users.</p>\u0000 </section>\u0000 </div>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"15 10","pages":"1257-1269"},"PeriodicalIF":2.9,"publicationDate":"2023-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9096465","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}