Regulatory control of glycopyrrolate in performance horses using validated UHPLC/MS–MS methods

Rumpler, M. J.; Samś, R. A.; Colahan, Patrick T.

doi:10.1016/j.jchromb.2012.02.008

Cited by 8 publications

(6 citation statements)

References 22 publications

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“…257 Glycopyrrolate belongs to the group of anticholinergic drugs, and it is a peripheral antimuscarinic agent used in a variety of clinical applications, such as treatment of chronic obstructive pulmonary disease and as a preanesthetic agent to reduce secretions. 261 Glycopyrrolate is considered a doping drug; therefore, analytical methods were developed for its detection in horse plasma 262 and horse urine, 263 both by LC-MS.…”

Section: Bronchodilatorsmentioning

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: Bronchodilatorsmentioning

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

“…Indeed, most recent studies utilizing SPE have found success with weak cation exchange or mixed mode cation exchange sorbents. 22,26,27,29,[40][41][42] During our initial method development, we compared the Evolute Express WCX cartridge to the Isolute weak cation exchange CBA cartridge (Biotage) to determine which cartridge would provide optimal results. The results from our preliminary method development data suggested that the CBA cartridge provided comparable results with the WCX for the QADs, but the WCX was superior for the monitored peptides.…”

Section: Sample Processing and Solid-phase Extractionmentioning

confidence: 99%

Detection of doping peptides and basic drugs in equine urine using liquid chromatography–mass spectrometry

Flores,

Hargrave,

Clifford

et al. 2023

Drug Testing and Analysis

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The abuse of prohibited agents including peptides and basic small‐molecule drugs is an area of great concern in horseracing due to their high potential to act as doping agents. These compound classes include agents such as growth hormone‐releasing peptides, peptide analgesics, beta‐2‐adrenergic receptor agonists, and quaternary ammonium drugs that can be challenging to detect and regulate because of their chemical properties and potential rapid elimination following administration. The use of highly sensitive and selective analytical techniques such as liquid chromatography–mass spectrometry (LC–MS) is necessary to provide coverage of these substances and their potential metabolites. This study describes the development and validation of methodology capable of the detection of over 50 different peptide‐based doping agents, related secretagogues, quaternary ammonium drugs, and other challenging small molecules in equine urine following solid‐phase extraction using a mixed mode weak cation exchange sorbent. Following sample extraction, the compounds were analyzed using LC–MS with chromatographic separation via a reverse phase gradient and detection via selective reaction monitoring following introduction to a triple‐stage quadrupole mass spectrometer using positive mode electrospray ionization. Validation parameters including limits of detection and quantitation, accuracy, precision, linear range, recovery, stability, and matrix effects were determined. Briefly, the limits of detection for most compounds were in the sub‐ng/mL ranges with adequate precision and accuracy sufficient for an initial testing procedure. Stability studies indicated that most compounds were sufficiently stable to allow for effective screening using conditions commonly utilized in drug testing laboratories.

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“…Glycopyrrolate is an official drug in Indian Pharmacopoeia [21] and United States Pharmacopoeia [22]. HPLC with UV detection [23,24], HPTLC with densitometry [25], ESI-LC-MS/MS [26], UHPLC-MS/MS [27] [28], GC-MS [29] and capillary electrophoresis [30] techniques are found in the literature for the quantification of glycopyrrolate in bulk, pharmaceutical dosage forms, human plasma, horse urine and plasma and equine urine.…”

Section: Simultaneous Quantification Of Formoterol Fumarate and Glycomentioning

confidence: 99%

Simultaneous Quantification of Formoterol Fumarate and Glycopyrrolate Using Reverse Phase High Performance Liquid Chromatography

Kalaiselvan¹,

Rajarathinam²,

Chandran³

2018

Asian J. Chem.

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A fully validated and rapid RP-HPLC method suitable for the quantification of formoterol fumarate and glycopyrrolate combination is reported. Chromatographic separation was achieved on a Sunsil C18 analytical column (250 mm × 4.6 mm, 5 µ particle size). The analytes were detected and quantified by photodiode array detector set at 289 nm. Calibration curves were constructed in the range of 4.8-14.4 µg/ mL (R 2 = 0.9997) with a limit of quantification of 0.279 µg/mL for formoterol fumarate and 9-27 µg/mL (R 2 = 0.9998) with a limit of quantification 0.239 µg/mL for glycopyrrolate. The method was validated aaccording to ICH guidelines. The developed and validated RP-HPLC method was sensitive, selective, robust, accurate and precise for the simultaneous estimation of formoterol fumarate and glycopyrrolate in quality control laboratories.

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Regulatory control of glycopyrrolate in performance horses using validated UHPLC/MS–MS methods

Cited by 8 publications

References 22 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

Detection of doping peptides and basic drugs in equine urine using liquid chromatography–mass spectrometry

Simultaneous Quantification of Formoterol Fumarate and Glycopyrrolate Using Reverse Phase High Performance Liquid Chromatography

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