• Title/Summary/Keyword: Equine urine

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Quantification of Three Prohibited Anabolic-Androgenic Steroids in Equine Urine using Gas Chromatography-Tandem Mass Spectrometry

  • Young Beom Kwak;Shaheed Ur Rehman;Hye Hyun, Yoo
    • Mass Spectrometry Letters
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    • v.14 no.3
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    • pp.104-109
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    • 2023
  • Anabolic-androgenic steroids (AAS) are used illegally to enhance muscle development and increase strength and power. In this study, a reliable, and sensitive quantitative method was developed and validated using heptafluorobutyric acid anhydride (HFPA) derivatives for the simultaneous detection of prohibited AAS (testosterone [TS], boldenone [BD], 5α-estrane-3β,17α-diol [EAD]) using gas chromatography-tandem mass spectrometry (GC-MS/MS). For processing the samples, solid phase extraction, methanolic hydrolysis, and liquid-liquid extraction were used. For detection using mass spectrometry, the multiple reaction monitoring (MRM) mode was used with the electron ionization (EI) positive mode. The method was evaluated for selectivity, linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and stability. The results showed that the method was accurate and reproducible for the quantitation of the three steroids. The developed method was finally applied to the analysis of a suspect gelding urine sample received from the Asian Quality Assurance Program (AQAP).

Simultaneous Analysis of Several Non-Steroidal Anti-Inflammatory Drugs in Urine by Gas Chromatograph/Negative Chemical Ionization-Mass Spectrometry (기체 크로마토그래프-질량분석법을 이용한 뇨중 비스테로이드성 소염진통제 (NSAIDs)의 동시 분석법)

  • Myung, Seung-Woon;Park, Joon-Ho;Kim, Myung-Soo;Cho, Hyun-Woo
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.571-576
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    • 1999
  • Screening method for NSAIDs (Hon-Steroidal Anti-Inflammatory Drugs) in urine was developed using GC/NCI-MS. Derivatized six fenamates with pentafluoropropionic anhydride showed high sensitivity in NCI-MS. The conditions of the derivatization reaction and chromatographic conditions were established for screening with a trace analysis. Limit of detection was in the range of 4-25 pg/mL. This method may be used to the equine doping analysis for NSAIDs and forensic analysis.

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Optimization of solid-phase extraction for the liquid chromatography-tandem mass spectrometry analysis of basic drugs in equine urine (액체크로마토그래피-텐덤질량분석법을 위한 경주마 소변 중 염기성 약물의 고체상 추출법 최적화)

  • Shin, Hyun Du;Yang, Ji Suk;Jung, Mihye;Kim, Hyung-Seung;Youm, Jeong-Rok;Hu, Man Bae;Kim, Sung Jean;Han, Sang Beom
    • Analytical Science and Technology
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    • v.21 no.5
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    • pp.412-423
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    • 2008
  • A procedure based on solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of 55 basic drugs in equine urine. The test scope covers diversified classes of drugs including some ${\beta}$-blockers, ${\beta}$-agonists, antihypotensives, CNS stimulants, sedatives, tranquilizers, antidepressants, antihypertensives and so on. LC-MS/MS separation and quantification was carried out in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Four different brands of mixed mode cation exchange SPE sorbents; UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$ and Waters Oasis$^{(R)}$ MCX were compared. The UCT XTRACT$^{(R)}$ XRDAH sorbent provided the best results in the preconcentration of samples, yielding relative recoveries higher than 80% except for terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%). Detection limits of the target drugs provided by the proposed analytical procedure were between 0.2~8.3 ng/mL.

Prevalence of Detection of Prohibited Drugs on Doping Tests of Pre- and Post-races in Korea (2002-2013) (국내 경주마 도핑검사에서 금지약물 검출빈도 및 종류(2002-2013))

  • Yang, Jaehyuk;Han, Kwan-Seok;Yang, Young-Jin;Lim, Yoon-Kyu
    • Journal of Veterinary Clinics
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    • v.32 no.2
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    • pp.215-217
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    • 2015
  • There was no study on the prevalence of doping control of racehorses in Korea. The purpose of this study was to determine prohibited substances in horse races of a drugs testing program. Blood samples were taken from those 298,543 starters prior to racing and the that finished top 3 runners of each race and horses designated by the stewards shall be taken for collection of 91,482 urine samples for the purpose of post-race doping test in Seoul, Busan and Jeju Race Park between 2002 and 2013. Detection and measurement of prohibited substances were carried out by ELISA, GC/MS and LC/MS using standard methods at the Doping Control Center, Korea Racing Authority. Total 0.0030% of pre-races and total 0.0186% of post-races tested positive for prohibited substances. In pre- and post-race, caffeine and ketoprofen were the most detected prohibited substance respectively. We thought that characteristics of pharmacokinetics and pharmacodynamics of drugs resulted in different between plasma and urine. These substances have also been detected with other prohibited drugs suggesting that unintentional feeding or bedding may be the reason and groomers' confusion of candidate horses based by the stewards' research.