Alisha Henderson, Liam M. Heaney, Stephanie Rankin-Turner
{"title":"Ambient ionisation mass spectrometry for drug and toxin analysis: A review of the recent literature","authors":"Alisha Henderson, Liam M. Heaney, Stephanie Rankin-Turner","doi":"10.1002/dta.3644","DOIUrl":"10.1002/dta.3644","url":null,"abstract":"<p>Ambient ionisation mass spectrometry (AIMS) is a form of mass spectrometry whereby analyte ionisation occurs outside of a vacuum source under ambient conditions. This enables the direct analysis of samples in their native state, with little or no sample preparation and without chromatographic separation. The removal of these steps facilitates a much faster analytical process, enabling the direct analysis of samples within minutes if not seconds. Consequently, AIMS has gained rapid popularity across a diverse range of applications, in particular the analysis of drugs and toxins. Numerous fields rely upon mass spectrometry for the detection and identification of drugs, including clinical diagnostics, forensic chemistry, and food safety. However, all of these fields are hindered by the time-consuming and laboratory-confined nature of traditional techniques. As such, the potential for AIMS to resolve these challenges has resulted in a growing interest in ambient ionisation for drug and toxin analysis. Since the early 2000s, forensic science, diagnostic testing, anti-doping, pharmaceuticals, environmental analysis and food safety have all seen a marked increase in AIMS applications, foreshadowing a new future for drug testing. In this review, some of the most promising AIMS techniques for drug analysis will be discussed, alongside different applications of AIMS published over a 5-year period, to provide a summary of the recent research activity for ambient ionisation for drug and toxin analysis.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"16 11","pages":"1323-1344"},"PeriodicalIF":2.6,"publicationDate":"2024-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/dta.3644","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139701379","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}
Carmel E. Heiland, Mikael Lehtihet, Annica Börjesson, Lena Ekström
{"title":"Evaluation of a single Eporatio® micro-dose in urine and dried blood spots","authors":"Carmel E. Heiland, Mikael Lehtihet, Annica Börjesson, Lena Ekström","doi":"10.1002/dta.3651","DOIUrl":"10.1002/dta.3651","url":null,"abstract":"<p>Recombinant human erythropoietin (rhEPO) has been abused as a performance enhancer in sports for several years, but with advancements in detection methods, even micro-doses can be detected in dried blood spot (DBS) samples. Here, we present the results from an Eporatio® (epoetin theta) micro-dose administration study to detect rhEPO in DBS samples. Five healthy male volunteers received a 15 IU/kg subcutaneous dose of Eporatio®. Urine and DBS samples (Mitra® VAMS and Capitainer® B50) were collected 1, 10, 24, 36, 48 and 72 h after drug administration. After 1 h, all urine samples were negative for rhEPO, whereas 40% of DBS samples were considered suspicious. All samples between 10 and 48 h were suspicious for the presence of Eporatio®, except one urine sample that was negative at 48 h. After 72 h, 40% of urine samples and 60% of DBS samples were suspicious and would have proceeded to a confirmation analysis. DBS is an efficient complementary matrix to urine for detection of rhEPO micro-doses.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"16 11","pages":"1319-1322"},"PeriodicalIF":2.6,"publicationDate":"2024-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/dta.3651","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139696583","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}
Abuelgasim Elrasheed, Simon Elliott, Muneeb Venayikot, Thomas Keller
{"title":"Synthetic cannabinoid detection in patients admitted for drug rehabilitation in the United Arab Emirates","authors":"Abuelgasim Elrasheed, Simon Elliott, Muneeb Venayikot, Thomas Keller","doi":"10.1002/dta.3653","DOIUrl":"10.1002/dta.3653","url":null,"abstract":"<p>This paper describes the investigation of synthetic cannabinoid news psychoactive substances in drug rehabilitation patients in the UAE. This represents the latest data for such drugs in the Gulf region.\u0000\u0000 <figure>\u0000 <div><picture>\u0000 <source></source></picture><p></p>\u0000 </div>\u0000 </figure></p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"16 11","pages":"1312-1318"},"PeriodicalIF":2.6,"publicationDate":"2024-02-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139690832","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}
Francesco Donati, Alice Natalucci, Livia Concetti, Xavier de la Torre, Francesco Botrè
{"title":"A SNP-based genotyping strategy to detect the abuse of homologous blood transfusion from dried blood spots","authors":"Francesco Donati, Alice Natalucci, Livia Concetti, Xavier de la Torre, Francesco Botrè","doi":"10.1002/dta.3650","DOIUrl":"10.1002/dta.3650","url":null,"abstract":"<p>We performed genotyping analysis of human biallelic polymorphisms (single nucleotide polymorphisms) for the detection of homologous blood transfusion in sports doping. DNA was extracted from dried blood spots and quantified real-time fast PCR. The method was proven to allow the detection of transfusions up to a donor percentage of 1%, with a significant improvement in terms of sensitivity with respect to both the reference cytofluorimetric method and a previously proposed strategy based on the DNA STR-based strategy.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"16 11","pages":"1306-1311"},"PeriodicalIF":2.6,"publicationDate":"2024-01-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/dta.3650","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139641315","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}
Evsen Yavuz Guzel, Aslı Atasoy Aydin, İsmail Ethem Gören, Necdet Unuvar, Nebile Daglioglu
{"title":"Estimation of anti-diabetes drug metformin in Turkiye using wastewater-based epidemiology","authors":"Evsen Yavuz Guzel, Aslı Atasoy Aydin, İsmail Ethem Gören, Necdet Unuvar, Nebile Daglioglu","doi":"10.1002/dta.3646","DOIUrl":"10.1002/dta.3646","url":null,"abstract":"<p>Metformin is the most commonly used drug for the treatment of type 2 diabetes (T2D), which is dramatically increasing due to factors such as increasing obesity, physical inactivity, and aging of the population. Metformin analysis was carried out in composite wastewater samples seasonally collected from wastewater treatment plants in 10 cities in 2019 and 2020 30 cities in 2021 in Turkiye. Metformin was measured in all wastewater samples, with an average concentration of 97.81 μg/l in 2019, 75.19 μg/l in 2020, and 69.13 μg/l in 2021. This study was utilized to predict metformin usage in different sociodemographic regions in Turkiye using a wastewater-based epidemiology (WBE) approach. As a result of the analysis, the average metformin consumption in Turkiye was estimated to be 22.2 ± 9.6 [1.9–63.8] g/d/1,000 persons (mean ± SD [range]). Furthermore, these estimates were compared with data for time, sociodemographic characteristics, and patient numbers. Assessing the correlation with estimates and the socioeconomic classes of the cities in question revealed that cities with high-income levels had the lowest metformin use rate. Finally, the study provides supporting data aiding the development of public health strategies for decreasing the overall load of T2D across Turkiye.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"16 11","pages":"1295-1305"},"PeriodicalIF":2.6,"publicationDate":"2024-01-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139666565","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}
Bastien Krumm, Carsten Lundby, Joar Hansen, Jacob Bejder, Henrik Sørensen, Tristan Equey, Jonas Saugy, Francesco Botrè, Raphael Faiss
{"title":"Yearly intrasubject variability of hematological biomarkers in elite athletes for the Athlete Biological Passport","authors":"Bastien Krumm, Carsten Lundby, Joar Hansen, Jacob Bejder, Henrik Sørensen, Tristan Equey, Jonas Saugy, Francesco Botrè, Raphael Faiss","doi":"10.1002/dta.3645","DOIUrl":"10.1002/dta.3645","url":null,"abstract":"<p>Confounding factors including exercise and environments challenge the interpretation of individual Athlete Biological Passports (ABPs). This study aimed to investigate the natural variability of hematological ABP parameters over 1 year in elite athletes compared with healthy control subjects and the validity of a multiparametric model estimating plasma volume (PV) shifts to correct individual ABP thresholds. Blood samples were collected monthly with full blood counts performed by flow cytometry (Sysmex XN analyzers) in 20 elite xc-skiers (ELITE) and 20 moderately trained controls. Individual ABP profiles were generated through Anti-Doping Administration & Management System Training, a standalone version of the ABP's adaptive model developed by the World Anti-Doping Agency. Additionally, eight serum parameters were computed as volume-sensitive biomarkers to run a multiparametric model to estimate PV. Variability in ELITE compared with controls was significantly higher for the Abnormal Blood Profile Scores (<i>P</i> = 0.003). Among 12 Atypical Passport Findings (ATPF) initially reported, six could be removed after correction of PV shifts with the multiparametric modeling. However, several ATPF were additionally generated (<i>n =</i> 19). Our study outlines a larger intraindividual variability in elite athletes, likely explained by more frequent exposure to extrinsic factors altering hematological biomarkers. PV correction for individual ABP thresholds allowed to explain most of the atypical findings while generating multiple new ATPF occurrences in the elite population. Overall, accounting for PV shifts in elite athletes was shown to be paramount in this study outlining the opportunity to consider PV variations with novel approaches when interpreting individual ABP profiles.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"16 11","pages":"1285-1294"},"PeriodicalIF":2.6,"publicationDate":"2024-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/dta.3645","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139641316","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}
Olga V. Kupriyanova, Vadim A. Shevyrin, Raziya G. Sadykova, Yuri M. Shafran
{"title":"Identification of thermolabile positional isomers of N-(2-hydroxybenzyl)-2-(dimethoxyphenyl)ethanamines (NBOH series) using chromatography and mass spectrometry methods","authors":"Olga V. Kupriyanova, Vadim A. Shevyrin, Raziya G. Sadykova, Yuri M. Shafran","doi":"10.1002/dta.3648","DOIUrl":"10.1002/dta.3648","url":null,"abstract":"<p>Among <i>N</i>-((2-substituted)benzyl)phenylethanamines, <i>N</i>-(2-hydroxybenzyl)phenylethanamines are a special type of compounds which are thermolabile and degrade in the course of analysis by means of gas chromatography–mass spectrometry (GC–MS). This can lead to substantial errors, in the identification of legally controlled compounds of this series containing methoxy groups at positions 2 and 5 of the benzene ring of the phenylethyl fragment by GC–MS, which is commonly used in forensic and toxicological laboratories. Exemplified by the five isomeric 2-(dimethoxyphenyl)-<i>N</i>-(2-hydroxybenzyl)ethanamines, it was shown that their derivatization with trifluoroacetic anhydride (same as in the case of the <i>N</i>-(2-methoxybenzyl)-, <i>N</i>-(2-fluorobenzyl)-, <i>N</i>-(2-chlorobenzyl)-, and <i>N</i>-(2-bromobenzyl)substitutes phenylethanamines [NBOMe, NBF, NBCl, and NBBr, respectively] series described earlier) results in only one product, <i>N</i>-monosubstituted derivative, for each positional isomer within a series, which makes it possible to reliably identify each compound by the GC–MS method. In addition, chromatographic conditions for sufficient separation of trifluoroacetyl derivatives of these positional isomers of the NBOH series in 25 min are proposed, which is an important aspect for analysis in forensic laboratories engaged in the determination of narcotic drugs and new psychoactive substances. As an alternative approach, a method for identifying positional isomers of the NBOH series by the high-performance liquid chromatography–high-resolution mass spectrometry (HPLC-HRMS) method without derivatization is proposed.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"16 11","pages":"1271-1284"},"PeriodicalIF":2.6,"publicationDate":"2024-01-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139541264","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}
Anca Frinculescu, Trevor Shine, John Ramsey, Lewis Couchman, Nunzianda Frascione, Vincenzo Abbate
{"title":"Analysis of drugs seized from amnesty bins at two major United Kingdom summer music festivals using two portable gas chromatography-mass spectrometry (GC–MS) instruments","authors":"Anca Frinculescu, Trevor Shine, John Ramsey, Lewis Couchman, Nunzianda Frascione, Vincenzo Abbate","doi":"10.1002/dta.3629","DOIUrl":"10.1002/dta.3629","url":null,"abstract":"<p>Globally, the number of drug users and the proportion of the drug using population has increased from 210 million in 2009 to 269 million in 2019. Several studies suggest that music festival attendees are more likely to abuse illicit substances and have a high-risk profile. Consequently, it is crucial to develop robust field drug analysis methods that facilitate harm reduction and drug monitoring. The work presented in this report aimed at developing and validating qualitative analytical methods for 3,4-methylenedioxymethamphetamine, 4-bromo-2,5-dimethoxyphenethylamine (2C-B), ketamine and <i>N</i>-ethylpentylone on two portable gas chromatography–mass spectrometry (GC–MS) systems: Griffin G510 (Teledyne FLIR, West Lafayette, IN) and Torion T-9 (PerkinElmer, Shelton, CT). The diagnostic ability of the mobile GC–MS units was assessed on 200 samples in total, seized at two large summer music festivals in the United Kingdom. The method validation process included selectivity/specificity, limit of identification, carry-over, ruggedness/robustness, and inter- and intra-day precision (repeatability and reproducibility). The Griffin G510 demonstrated a limit of identification from 1 mg/mL for 2C-B to 0.063 mg/mL for ketamine and good ruggedness and precision results. The precision for 2C-B using the Torion T-9 was poorer than for the Griffin G510, but equivalent for the other compounds tested. Correct identifications (versus benchtop GC–MS) for the two festivals were 85%–86% and 74%–83% for the Griffin G510 and the Torion T-9, respectively. The two portable instruments were able to adequately cover current on-site drug-testing analytical gaps and proved to be a powerful addition to the on-site drug analysis techniques.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"16 11","pages":"1241-1253"},"PeriodicalIF":2.6,"publicationDate":"2024-01-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/dta.3629","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139541258","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}
Kathrine Skov, Sys Stybe Johansen, Kristian Linnet, Marie Katrine Klose Nielsen
{"title":"Automated enzymatic hydrolysis of urine samples for improved systematic toxicological analysis of drug-facilitated sexual assault cases","authors":"Kathrine Skov, Sys Stybe Johansen, Kristian Linnet, Marie Katrine Klose Nielsen","doi":"10.1002/dta.3640","DOIUrl":"10.1002/dta.3640","url":null,"abstract":"<p>Drug-facilitated sexual assault (DFSA) is characterized by victim incapacitation due to intoxicating substances. Detection of single drug exposure from DFSA requires a systematic toxicological analysis strategy including sensitive methods covering a broad spectrum of substances. The aim of this study was to develop and validate an UHPLC–MS/MS screening method for analysis of samples from DFSA cases and incorporate an automated enzymatic pre-treatment of urine samples into a robotic sample preparation for an efficient laboratory workflow. The screening method included 144 drugs of abuse, pharmaceuticals, and metabolites relevant to DFSA. The use of a recombinant enzyme showed an efficient glucuronide hydrolysis with an average parent drug recovery of 97%. Investigation of matrix effect showed no pronounced ion enhancement or suppression for most analytes (96%), and extraction recovery was above 80% for 97% of analytes. Process efficiency ranged from 50% to 138% for most analytes. The LODs ranged from 0.0001 mg/L to 2 mg/L depending on analyte, and most analytes met the SOFT recommended minimum performance limits. The validated method was applied to authentic suspected DFSA cases (<i>n</i> = 38). Results showed that drugs of abuse, benzodiazepines, and antidepressants were most commonly found in suspected DFSA cases. Incorporation of an automated enzymatic hydrolysis step during sample preparation enables a fast and simple workflow for simultaneous analysis of blood and urine samples for an improved systematic toxicological analysis strategy for DFSA cases.</p>","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"16 11","pages":"1254-1270"},"PeriodicalIF":2.6,"publicationDate":"2024-01-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/dta.3640","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139541261","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":"Interest of nail clipping tests to discriminate a tail end of a doping regimen from a contamination in case of challenging an adverse analytical finding: Case reports involving ostarine","authors":"Pascal Kintz, Laurie Gheddar, Alice Ameline","doi":"10.1002/dta.3577","DOIUrl":"10.1002/dta.3577","url":null,"abstract":"","PeriodicalId":160,"journal":{"name":"Drug Testing and Analysis","volume":"16 5","pages":"515-517"},"PeriodicalIF":2.9,"publicationDate":"2023-09-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10634611","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}