High-throughput screening of corticosteroids and basic drugs in horse urine by liquid chromatography-tandem mass spectrometry

Leung, Gary N. W.; Chung, Evonne W.; Ho, Emmie N.M.; Kwok, Wai‐Him; Leung, David K.K.; Tang, Fei; Wan, Terence S.M.; Yu, Nola H.

doi:10.1016/j.jchromb.2004.12.039

Cited by 36 publications

(31 citation statements)

References 16 publications

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“…[104] Moreover, a comprehensive screening methodology has been developed and includes a single deconjugation procedure with a solution of protease and β-glucuronidase, and separate collection of basic and acidic/neutral fractions after SPE with mixed mode C8-cartridge. [105,106] Furthermore, a unified sample preparation procedure has been established that combines different deconjugation, extraction, and derivatization procedures. [107] It begins with two parallel procedures which include (1) enzymatic hydrolysis of sulfate and glucuronide conjugates (β-glucuronidase and arylsulfatase) and (2) methanolysis of the 17β-sulfate steroid conjugates.…”

Section: Horse Urine Samplesmentioning

confidence: 99%

“…Recently, hydrophilic interaction chromatography (HILIC) has become the technique preferred for the analysis of polar and ionizable compounds, [114][115][116] as occurred in the detection of myo-inositol trispyrophosphate (ITPP) in equine urine and plasma which is a new drug, capable of increasing the amount of oxygen in hypoxic tissues and is an ideal candidate as doping agent in racehorses. [117,118] LC-MS instruments equipped with mass analyzers with MS/MS capabilities, such as triple quadrupole (QqQ) [104][105][106]108] and triple quadrupole/linear ion trap (QTrap), [101,106,110,112,119] have been implemented successfully in common screening methods in equine doping control. These LC-MS/MS systems provide analyses with high sensitivity and specificity which are critical prerequisites for the detection of banned compounds in trace concentration levels in complex biological samples.…”

Section: Mass Spectrometric Techniques In the Equine Doping Controlmentioning

confidence: 99%

“…[105] • Forty anabolic steroids and corticosteroids using MRM in positive ESI mode and 52 acidic dugs using MRM in negative ESI mode, through fast-scanning MS with only 10 min overall turnaround times for both methods because of the high efficiency RP-column utilized. [106] • One hundred forty multiclass drugs in a single 13 min run through a UPLC column coupled with a fast scanning and fast ESI polarity switching tandem MS in SRM mode.…”

Section: Mass Spectrometric Techniques In the Equine Doping Controlmentioning

confidence: 99%

See 2 more Smart Citations

Challenges in detecting substances for equine anti‐doping

Fragkaki

Kioukia‐Fougia

Kiousi

et al. 2017

Drug Testing and Analysis

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The artificial increase of the physical capability of horses using drugs is well known in racing and other equine sports. Both illicit and therapeutic substances are regarded as prohibited substances in competition in most countries. Some countries make distinctions for a few, specific drugs which are, however, allowed for use in other countries. The primary objective in the case of doping control is the detection of any trace of drug exposure, either parent drug or any of its metabolites, using the most powerful analytical methods which are generally based on chromatographic/mass spectrometric techniques. Of major concern in horseracing is the absence of a single organization regulating the anti-doping framework; instead of this, individual racing authorities provide rules and regulations often resulting in variations in the applied doping control programmes of different countries. The aim of this paper is to review the recent literature (approximately from 2012 to mid-2016) to highlight the numerous and diverse challenges faced in doping control of racing and equestrian sports, including the detection of designer drugs (anabolic steroids or stimulants) and of other emerging prohibited substances, such as peptides and noble gases in horse urine and plasma. Moreover, the application of 'omics' techniques (especially of metabolomics) deserves attention for establishing possible fingerprints of drug abuse as well as the evolution of instrumental analysis resulting a powerful ally in the fight against doping in equine sports.

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Section: Horse Urine Samplesmentioning

confidence: 99%

Section: Mass Spectrometric Techniques In the Equine Doping Controlmentioning

confidence: 99%

Section: Mass Spectrometric Techniques In the Equine Doping Controlmentioning

confidence: 99%

See 1 more Smart Citation

Challenges in detecting substances for equine anti‐doping

Fragkaki

Kioukia‐Fougia

Kiousi

et al. 2017

Drug Testing and Analysis

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“…AT was determined in urine [16] and in plasma [17 -21] by LC, while CT was determined in urine by GC [22,23]. Both AT and CT were determined in plasma by HPLC [24].…”

Section: Introductionmentioning

confidence: 99%

HPLC method for the simultaneous determination of atenolol and chlorthalidone in human breast milk

El‐Gindy

Sallam

Salam³

2008

J of Separation Science

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A high-performance liquid chromatographic method was optimized and validated for the determination of atenolol and chlorthalidone (CT) in human breast milk. The milk samples were extracted and purified using ACN and phosphoric acid for precipitation of proteins followed by removal of ACN and milk fats by extraction with methylene chloride. The samples were applied, after an extraction procedure, to a cyanide column using a mobile phase consisting of ACN/water (35:65 v/v) and buffered at pH 4.0 with flow rate of 1.0 mL/min. Quantitation was achieved with UV detection at 225 nm using guaifenesin as the internal standard. The effectiveness of protein precipitation and clean up procedure were investigated. The method was validated over the range of 0.3-20 microg/mL for atenolol and 0.25-5 microg/mL for CT.

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“…This structural difference leads to the four-fold higher glucocorticoid or anti-inflammatory activity of prednisolone compared to the activity of cortisol, [2] and therefore it is a drug commonly utilised in veterinary practice, with topical or systemic uses. [3][4][5] As with other corticosteroids, prednisolone can however be abused in equine sports to increase athlete horse performance, [6,7] so it is classified as a prohibited substance. [8] A thorough review of the literature regarding the detection of prednisolone in equine biological matrices (urine, plasma) suggests that this corticosteroid presents some difficulties in analysis, especially when is present at low concentrations, due to interfering substances.…”

mentioning

confidence: 99%

Investigation of the presence of endogenous prednisolone in equine urine by high‐performance liquid chromatography mass spectrometry and high‐resolution mass spectrometry

Fidani

Pompa

Mungiguerra

et al. 2012

Rapid Comm Mass Spectrometry

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The very high frequency of prednisolone detection in the samples (78.5%), the low concentration of this steroid and, importantly, the narrow range of the 95% confidence limits (0.97-1.05 in MS(2) mode and 0.88-1.04 in MS(3) mode), could represent evidence that its presence is endogenous. In the light of these results, this hypothesis seems the most probable, even if further studies are required to confirm it. Furthermore, a microbiological origin (i.e. fermentation of cortisol after sample collection) could not be disregarded.

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High-throughput screening of corticosteroids and basic drugs in horse urine by liquid chromatography-tandem mass spectrometry

Cited by 36 publications

References 16 publications

Challenges in detecting substances for equine anti‐doping

Challenges in detecting substances for equine anti‐doping

HPLC method for the simultaneous determination of atenolol and chlorthalidone in human breast milk

Investigation of the presence of endogenous prednisolone in equine urine by high‐performance liquid chromatography mass spectrometry and high‐resolution mass spectrometry

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