Dried Urine Microsampling Coupled to Liquid Chromatography—Tandem Mass Spectrometry (LC–MS/MS) for the Analysis of Unconjugated Anabolic Androgenic Steroids

Protti, Michele; Marasca, Camilla; Cirrincione, Marco; Sberna, Angelo Eliseo; Mandrioli, Roberto; Mercolini, Laura

doi:10.3390/molecules25143210

Cited by 17 publications

(16 citation statements)

References 31 publications

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“…Another “construction area” in drug testing has been reduction of costs associated with sample transport and storage. Here, the potential of using dried microvolumes of urine was assessed, and 30 μl sampling devices were used to prepare dried urine spots for ultrasonication‐assisted extraction into methanol for subsequent LC‐MS/MS analysis 55 . Thirteen steroidal compounds including T, EpiT, DHEA, dihydrotestosterone (DHT), and other AAS were separated on a C‐18 LC column (50 × 2.1 mm, 2.7 μm particle size) with the organic solvent (acetonitrile containing 0.1% formic acid) as component A and the aqueous solvent (0.1% formic acid) as component B.…”

Section: Anabolic Agentsmentioning

confidence: 99%

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Annual banned‐substance review: Analytical approaches in human sports drug testing 2019/2020

Thevis

Kuuranne

Geyer

2020

Drug Testing and Analysis

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Analytical chemistry-based research in sports drug testing has been a dynamic endeavor for several decades, with technology-driven innovations continuously contributing to significant improvements in various regards including analytical sensitivity, comprehensiveness of target analytes, differentiation of natural/ endogenous substances from structurally identical but synthetically derived compounds, assessment of alternative matrices for doping control purposes, and so forth. The resulting breadth of tools being investigated and developed by anti-doping researchers has allowed to substantially improve anti-doping programs and data interpretation in general. Additionally, these outcomes have been an extremely valuable pledge for routine doping controls during the unprecedented global health crisis that severely affected established sports drug testing strategies. In this edition of the annual banned-substance review, literature on recent developments in antidoping published between October 2019 and September 2020 is summarized and discussed, particularly focusing on human doping controls and potential applications of new testing strategies to substances and methods of doping specified the World Anti-Doping Agency's 2020 Prohibited List.

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Section: Anabolic Agentsmentioning

confidence: 99%

“…Here, the potential of using dried microvolumes of urine was assessed, and 30 μl sampling devices were used to prepare dried urine spots for ultrasonication-assisted extraction into methanol for subsequent LC-MS/MS analysis. 55…”

Section: Initial Testing Procedures-comprehensive Screening and Metmentioning

confidence: 99%

Annual banned‐substance review: Analytical approaches in human sports drug testing 2019/2020

Thevis

Kuuranne

Geyer

2020

Drug Testing and Analysis

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“…These microsamples can be obtained using a range of specific devices and collection protocols [30]. Common collection technologies include traditional dried samples such as DBSs and advanced microsampling devices (commercially available devices optimised to collect a variety of biological media, including whole blood [31,32], whole blood separated into plasma [33] or serum [34], and urine [35]). Most of these devices require a small amount of capillary blood from a minor skin incision such as a prick [28], usually from a fingertip; however, other sites have been utilised, such as the arm [36].…”

Section: Introductionmentioning

confidence: 99%

Advanced Microsamples: Current Applications and Considerations for Mass Spectrometry-Based Metabolic Phenotyping Pipelines

et al. 2022

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Microsamples are collections usually less than 50 µL, although all devices that we have captured as part of this review do not fit within this definition (as some can perform collections of up to 600 µL); however, they are considered microsamples that can be self-administered. These microsamples have been introduced in pre-clinical, clinical, and research settings to overcome obstacles in sampling via traditional venepuncture. However, venepuncture remains the sampling gold standard for the metabolic phenotyping of blood. This presents several challenges in metabolic phenotyping workflows: accessibility for individuals in rural and remote areas (due to the need for trained personnel), the unamenable nature to frequent sampling protocols in longitudinal research (for its invasive nature), and sample collection difficulty in the young and elderly. Furthermore, venous sample stability may be compromised when the temperate conditions necessary for cold-chain transport are beyond control. Alternatively, research utilising microsamples extends phenotyping possibilities to inborn errors of metabolism, therapeutic drug monitoring, nutrition, as well as sport and anti-doping. Although the application of microsamples in metabolic phenotyping exists, it is still in its infancy, with whole blood being overwhelmingly the primary biofluid collected through the collection method of dried blood spots. Research into the metabolic phenotyping of microsamples is limited; however, with advances in commercially available microsampling devices, common barriers such as volumetric inaccuracies and the ‘haematocrit effect’ in dried blood spot microsampling can be overcome. In this review, we provide an overview of the common uses and workflows for microsampling in metabolic phenotyping research. We discuss the advancements in technologies, highlighting key considerations and remaining knowledge gaps for the employment of microsamples in metabolic phenotyping research. This review supports the translation of research from the ‘bench to the community’.

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“…After drying/storage at room temperature, the VAMS device tip can undergo extraction with different solvents or solvent mixtures by means of various extraction procedures [ 19 ]. The VAMS technology has been successfully applied to several analytical challenges, such as pharmacokinetics [ 20 ], therapeutic drug monitoring (TDM) [ 21 , 22 ] and analysis of drugs of abuse [ 23 , 24 ], and to different biological fluids [ 25 , 26 , 27 , 28 , 29 , 30 ]. VAMS has also been applied to the discovery of protein biomarkers [ 31 ] and to the determination of amino acids and organic acids in metabolomic approaches [ 32 ].…”

Section: Introductionmentioning

confidence: 99%

Volumetric Absorptive Microsampling (VAMS) for Targeted LC-MS/MS Determination of Tryptophan-Related Biomarkers

et al. 2022

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L-Tryptophan (TRP) metabolites and related biomarkers play crucial roles in physiological functions, and their imbalances are implicated in central nervous system pathologies and neurodegenerative diseases such as amyotrophic lateral sclerosis (ALS), Alzheimer’s disease, Parkinson’s disease, schizophrenia and depression. The measurement of TRP metabolites and related biomarkers possesses great potential to elucidate the disease mechanisms, aid preclinical drug development, highlight potential therapeutic targets and evaluate the outcomes of therapeutic interventions. An effective, straightforward, sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of 24 TRP-related compounds in miniaturised murine whole blood samples. Sampling and sample pretreatment miniaturisation were achieved thanks to the development of a volumetric dried blood microsampling approach. Volumetric absorptive microsampling (VAMS) allows the accurate sampling of microvolumes of blood with advantages including, but not limited to, minimal sampling invasiveness, logistical improvements, method sustainability in terms of solvents and energy consumption, and improvement of animal studies in the framework of the 3Rs (Replacement, Reduction and Refinement) principles on animal welfare. The VAMS-LC-MS/MS method exhibited good selectivity, and correlation coefficient values for the calibration curves of each analyte were >0.9987. The limits of quantitation ranged from 0.1 to 25 ng/mL. The intra- and inter-day precisions in terms of RSD were <9.6%. All analytes were stable in whole blood VAMS samples stored at room temperature for at least 30 days with analyte losses < 14%. The developed method was successfully applied to the analysis of biological samples from mice, leading to the unambiguous determination of all the considered target analytes. This method can therefore be applied to analyse TRP metabolites and related biomarkers levels to monitor disease states, perform mechanistic studies and investigate the outcomes of therapeutic interventions.

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Dried Urine Microsampling Coupled to Liquid Chromatography—Tandem Mass Spectrometry (LC–MS/MS) for the Analysis of Unconjugated Anabolic Androgenic Steroids

Cited by 17 publications

References 31 publications

Annual banned‐substance review: Analytical approaches in human sports drug testing 2019/2020

Annual banned‐substance review: Analytical approaches in human sports drug testing 2019/2020

Advanced Microsamples: Current Applications and Considerations for Mass Spectrometry-Based Metabolic Phenotyping Pipelines

Volumetric Absorptive Microsampling (VAMS) for Targeted LC-MS/MS Determination of Tryptophan-Related Biomarkers

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