Liquid chromatography electrospray ionization tandem mass spectrometry for the detection of mesocarb abuse in horse doping

Appolonova, Svetlana A.; Baranov, Pavel A.; Mesonzhnik, Natalia V.; Brazhnikova, Daria O.; Rodchenkov, G. M.

doi:10.1002/dta.345

Cited by 3 publications

(9 citation statements)

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“…Urine samples were collected before administration and then at least twice a day for up to 6 days' post‐administration. Some of these metabolites ( p ‐hydroxymesocarb, hydroxymesocarb, and dihydroxymesocarb), could be detected for as long as 90–120 h after administration, being therefore adequate targets for the screening of mesocarb 192 …”

Section: Resultsmentioning

confidence: 99%

Doping detection in animals: A review of analytical methodologies published from 1990 to 2019

Moreira

Carmo

Pinho

et al. 2021

Drug Testing and Analysis

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Despite the impressive innate physical abilities of horses, camels, greyhounds, or pigeons, doping agents might be administered to these animals to improve their performance. To control these illegal practices, anti‐doping analytical methodologies have been developed. This review compiles the analytical methods that have been published for the detection of prohibited substances administered to animals involved in sports over 30 years. Relevant papers meeting the search criteria that discussed analytical methods aiming to detect and/or quantify doping substances in animal biological matrices published from 1990 to 2019 were considered. A total of 317 studies were included, of which 298 were related to horses, demonstrating significant advances toward the development of doping detection methods for equine sports. However, analytical methods for the detection of doping agents in sports involving other species are lacking. Due to enhanced accuracy and specificity, chromatographic analysis coupled to mass spectrometry detection is preferred over immunoassays. Regarding biological matrices, blood and urine remain the first choice, although alternative biological matrices, such as hair and feces, have been considered. With the increasing number and type of drugs used as doping agents, the analytes addressed in the published papers are diverse. It is very important to continue to detect and quantify these drugs, recognizing those that are most frequently used, in order to punish the abusers, protect animals' health, and ensure a healthier and genuine competition.

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Section: Resultsmentioning

confidence: 99%

Doping detection in animals: A review of analytical methodologies published from 1990 to 2019

Moreira

Carmo

Pinho

et al. 2021

Drug Testing and Analysis

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show abstract

“…Despite the good ionization efficiencies for steroids with a conjugated keto‐ groups, steroids containing only hydroxy‐ groups or non‐conjugated keto‐ groups show poor ionization 5–7. For this latter group of compounds, monitoring losses of water or adduct ions such as [M + NH 4 ] + can be alternative 8–12…”

Section: Introductionmentioning

confidence: 99%

“…Due to the problems described above, different types of chemical modifications (derivatization) of steroid's molecules are used prior to the HPLC‐MS analysis 5, 11, 13, 14. Derivatization procedures are not essential in HPLC‐MS, but their implementation provides better ionization conditions to assure proper sensitivity and selectivity of the evaluated methods.…”

Section: Introductionmentioning

confidence: 99%

“…Derivatization procedures are not essential in HPLC‐MS, but their implementation provides better ionization conditions to assure proper sensitivity and selectivity of the evaluated methods. Unfortunately, nowadays there are no group derivatization reagents for both hydroxy‐ and keto‐ groups selective modification 5, 11…”

Section: Introductionmentioning

confidence: 99%

“…Thus, the main aim of this work was to show the potential use of complex picolinoyl and oxime derivatives formation with following HPLC‐MS/MS analysis not only to overcome the problem of ionization suppression and sensitivity limits but to cover the range of anabolic steroid that are problematic in free fraction (underivatized) HPLC‐MS analysis also 11, 12…”

Section: Introductionmentioning

confidence: 99%

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The potential use of complex derivatization procedures in comprehensive HPLC‐MS/MS detection of anabolic steroids

Baranov¹,

Appolonova²,

Rodchenkov³

2010

Drug Testing and Analysis

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The use of two separate derivatization procedures with the formation of oxime (hydroxyl ammonium pretreatment) and picolinoyl (mixed anhydride method) derivates of anabolic steroids following HPLC-MS/MS analysis was proposed. The main product ions of obtained derivatives for 21 anabolic steroids were evaluated and fragmentation pathways were compared.The analysis of MS/MS spectra for underivatized steroids versus oxime or picolinoyl derivatives showed that in case of analytes containing conjugated double bonds in sterane core all of the observed MS/MS spectra contained abundant product ions of diagnostic value. The implementation of derivatization procedures to such compounds is useful for upgrading sensitivity or selectivity of the evaluated method. On the other hand, MS/MS spectra of underivatized and oxime analytes without conjugated double bonds in sterane core produce spectra with large amounts of low abundant product ions. Picolinoyl derivatives formation leads to highly specific spectra with product ions of diagnostic value coupled with sensitive and selective analysis at the same time. The intra- and inter-group comparison analysis revealed that fragmentation pathways for underivatized steroids and correspondent oxime derivatives are similar.The obtained oxime and picolinoyl derivatives provided 10-15 times higher ESI response in the HPLC-ESI-MS-selected reaction monitoring (SRM) when compared to those of underivatized molecules in positive HPLC-ESI-MS mode.Due to the laborious sample preparation we suggest to use the performed strategy for confirmation analysis purposes, metabolic studies or while the identification of new steroids or steroid-like substances.

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Mass Spectrometric Characterization of Plasma Mebeverine Metabolites and Its Synthesis

Moskaleva¹,

Kuznetzov²,

Markin³

et al. 2019

PTQ

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Mebeverine is a musculotropic antispasmodic drug that is widely used in the treatment of irritable bowel syndrome. As an ester of mebeverine alcohol and veratric acid, mebeverin is quickly metabolized and is practically undetectable in blood plasma. The main goal of this work was establishing the structure of the main metabolites of mebeverin in human blood plasma. The study was conducted by time-of-flight mass spectrometry (LC-IT-TOF MS), metabolites of mebeverine were extracted from plasma with acetonitrile. When comparing chromatograms of blood plasma obtained before and after drug administration, four main peaks of metabolites were detected. To establish the structure of the compounds, mass spectra of the first and second order were taken. The first-order spectra were used to calculate the metabolite formula and the structure was determined from the fragmentation spectra, as well as by comparing the fragmentation spectra of mebeverine and its proposed metabolites. The proposed compounds were synthesized, and their structure was confirmed using NMR and chromatography-mass spectrometry. Four main metabolites were found in this study: desmethylmebeverine acid (DMAC), glucuronide product of DMAC (DMAC-Glu), mebeverine acid (MAC) and mebeverine alcohol (MAL). The results complement the available literature data about the veratric acid metabolism, urine, and microsomal studies. According to the data obtained, the main metabolite of mebeverine in the blood is DMAC. The concentration of MAC after mebeverine administration is almost ten times less than DMAC, the content of MAL and DMAC-Glu is insignificant, and probably does not affect the pharmacological effect of mebeverine. Therefore, the concentration of DMAC is the main parameter to be monitored in pharmacokinetics studies.

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Liquid chromatography electrospray ionization tandem mass spectrometry for the detection of mesocarb abuse in horse doping

Cited by 3 publications

References 9 publications

Doping detection in animals: A review of analytical methodologies published from 1990 to 2019

Doping detection in animals: A review of analytical methodologies published from 1990 to 2019

The potential use of complex derivatization procedures in comprehensive HPLC‐MS/MS detection of anabolic steroids

Mass Spectrometric Characterization of Plasma Mebeverine Metabolites and Its Synthesis

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