• Title/Summary/Keyword: Doping control

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Analysis of Glycerol with Isolation of Endogenous Interferences using "Dilute and Shoot" Strategy and High-Resolution Mass Spectrometry in Human Urine for Antidoping Testing

  • Kim, Yongseok;Min, Hophil;Sung, Changmin;Park, Ju-hyung;Son, Junghyun;Lee, Kang Mi;Kim, Ho Jun;Lee, Jaeick;Kwon, Oh-Seung;Kim, Ki Hun
    • Mass Spectrometry Letters
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    • v.7 no.4
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    • pp.111-115
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    • 2016
  • Glycerol was identified and isolated from endogenous interferences during analysis of human urine using high-resolution mass spectrometry (HRMS) for doping control. Urinary sample preparation was simple; the samples were diluted with an organic solvent and then analyzed using a liquid chromatography-mass spectrometry ("dilute and shoot" method). Although the interfering ion peaks were observed at the similar retention time of glycerol, the inference could be identified by isolation with HRMS and further investigation. Thus, creatinine was identified as the endogenous interference for glycerol analysis and it also caused ion suppression resulting in the decrease of glycerol signal. This study reports the first identification and efficient isolation of endogenous interferences in human urine for "dilute and shoot" method. The information about ion suppression could be novel to prevent overestimation or a false result for antidoping analysis.

LC-MS/MS Method for Simultaneous Analysis of Growth Hormone-Releasing Peptides and Secretagogues in Human Urine

  • Min, Hophil;Han, Boyoung;Sung, Changmin;Park, Ju-Hyung;Lee, Kang Mi;Kim, Ho Jun;Kim, Ki Hun;Son, Junghyun;Kwon, Oh-Seung;Lee, Jaeick
    • Mass Spectrometry Letters
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    • v.7 no.3
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    • pp.55-63
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    • 2016
  • Growth hormone (GH)-releasing peptides (GHRPs) and GH secretagogues (GHSs) are listed in the World Anti-Doping Agency (WADA) Prohibited List. In the present study, we developed and validated a method for the simultaneous analysis of seven GHRPs (alexamorelin, GHRP-1, -2, -4, -5, -6, and hexarelin) and three GHSs (anamorelin, ibutamoren, and ipamorelin) in human urine. Method validation was performed at minimum required performance levels specified by WADA technical documents (2 ng/mL) for all substances, and the method was validated with regard to selectivity (no interference), linearity (R2 > 0.9986), matrix effects (50.0%-141.2%), recovery (10.4%-100.8%), and intra- (2.8%-16.5%) and inter-day (7.0%-22.6%) precisions. The limits of detection for screening and confirmation were 0.05-0.5 ng/mL and 0.05-1 ng/mL, respectively.

Method for Screening and Confirming Meldonium in Human Urine by High-Resolution Mass Spectrometry and Identification of Endogenous Interferences for Anti-Doping Testing

  • Kim, Yongseok;Jeong, Dawon;Min, Hophil;Sung, Changmin;Park, Ju-hyung;Son, Junghyun;Lee, Kang Mi;Kim, Ho Jun;Lee, Jaeick;Kwon, Oh-Seung;Kim, Ki Hun
    • Mass Spectrometry Letters
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    • v.8 no.2
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    • pp.39-43
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    • 2017
  • Meldonium is a drug for treating ischemia by expanding the arteries but it can also enhance the performance of sports players. The World Anti-Doping Agency (WADA) has included it in the list of prohibited substances since 2016. Meldonium is one of the challenging substances for anti-doping testing because it is difficult to recover by general liquid-liquid or solid phase extraction due to its permanent charge and high polarity. Therefore, high-performance liquid chromatography (HPLC) is currently used by injecting a diluted urine sample (known as the "dilute-and-shoot" strategy). There is no loss of target compounds in the extraction/cleanup procedure but its high matrix effect could interfere in their separation or detection from the endogenous urinary compounds. We report a single method using high-resolution mass spectrometry that can be used for both screening and confirmation, which follows the "dilute-and-shoot" strategy. In this method, the endogenous compounds' interfering peaks in the mass spectrum are separated at a high resolution of FWHM 140,000, and the results are suitable for substance detection following the WADA guidelines. The interferences in the obtained mass spectrum of the urine matrix are identified as acetylcholine, lysine, and glutamine by further analysis and database searching. Validation of the method is performed in routine anti-doping testing, and the limit of detection is 50 ng/mL. This method uses simple sample preparation and a general reverse phase HPLC column, and it can be easily applied to other substances.

An Analysis Study on the Doping Intentions of Athletes using Stepwise Regression Analysis

  • Youn-Suk Han;Jong-Hwa Park
    • Journal of the Korea Society of Computer and Information
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    • v.28 no.5
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    • pp.171-177
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    • 2023
  • This study aims to provide useful information for prevention of doping by investigating and verifying relationships among demographic factors such as athletic career and experience of anti-doping education, controlled motivation, attitude toward anti-doping, perceived behavioral control factors and doping intentions to verify factors affecting doping intentions of domestic elite athletes based on the advance studies that have been carried out various theoretical approaches so far. Method: This study analyzed using SPSS 27.0 program. First, this study confirmed a multicollinearity problem by conducting Pearson's correlation analysis to examine correlation between variables. And this study conducted stepwise multiple linear regression to confirm how the variables affect doping intentions. Result: Study results show that all factors such as athletic career, experience of anti-doping education, controlled motivation, attitude toward anti-doping and perceived behavioral control have a significant impact on doping intentions, and this study verified significant impact by putting variables in order of each influence. As a result of verification, this study confirmed that controlled motivation has the greatest influence, and perceived behavioral control toward doping, experience of anti-doping education, attitude toward and athletic career came next in order.

Evaluation of the Genetic Toxicity of Synthetic Chemicals (II), a Pyrethroid Insecticide, Fenpropathrin

  • Ryu, Jae-Chun;Kim, Kyung-Ran;Kim, Hyun-Joo;Ryu, Eun-Kyoung;Lee, Soo-Young;Jung, Sang-Oun;Youn, Ji-Youn;Kim, Min-Hee;Kwon, Oh-Seung
    • Archives of Pharmacal Research
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    • v.19 no.4
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    • pp.251-257
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    • 1996
  • The detection of many synthetic chemicals used in industry that may pose a genetic hazard in our environment is subject of great concern at present. In this respect, the genetic toxicity of fenpropathrin ((RS)-.alpha.-cyano-3-phenoxybenzyl-2,2,3,3-tetramethyl cyclopropane carboxylate, CAS No.:39514-41-8), a pyrethroid insecticide, was evaluated in bacterial gene mutation system, chromosome aberration in mammalian cell system and in vivo micronucleus assay with rodents. In bacterial gene mutation assay, no mutagenicity of fenpropathrin (62-$5000\mug/plate$) was observed in Salmonella typhimurium TA 98, 100, 1535 and 1537 both in the absence and in the presence of S-9 metabolic activaton system. In mammalian cell system using chinese hamster lung fibroblast, no clastogenicity of fenpropathrin was also observed both in the absence and in the presence of metabolic activation system in the concentration range of $7-28\mug/ml$. And also, in vivo micronucleus assay using mouse bone marrow cells, fenpropathrin also revealed no mutagenic potential in the dose range of 27-105 mg/kg body weight of fenpropathrin (i.p.). Consequently, no mutagenic potential of fenpropathrin was observed in vitro bacterial, mammalian mutagenicity systems and in vivo micronucleus assay in the dose ranges used in this experiment.

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Effect of Recombinant Bovine Somatotropin (${\gamma}$ bST) Administration on bST Levels in Milk of Cows

  • Park, Jeongeun;Park, Myung-Ja;Jaeho Chin;Park, Jongsei;Kim, Jooho
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1995.04a
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    • pp.127-127
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    • 1995
  • The present study was conducted to examine the effect of recombinant bovine somatotropin(${\gamma}$ bST), which was administered to cow to promote milk production, on bST levels in milk. Fourteen cows were divided into two groups: 1) control cows received neither y bST nor vehicle, 2) treated cows were administered twice at two-week interval with 500mg ${\gamma}$ bST each cow by subcutaneous injection. Milk samples were taken on day 0 (prior to injection), day 7 (7 days after 1st injection), day 21 (7 days after 2nd injection) and day 35 (21 days after 2nd injection).

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Simultaneous Analysis of Stimulants and Narcotic Analgesics by Capillary Column Gas Chromatography with Nitrogen Phosphorus Detector (Capillary Column Gas Chromatography/Nitrogen Phosphorus Detector를 이용한 흥분제 및 마약성 진통제의 동시분석에 관한 연구)

  • Lho, Dong-Seok;Shin, Ho-Sang;Kang, Bo-Kyung;Paek, Heang-Kee;Kim, Seung-Ki;Lee, Jeong-Ae;Kim, Young-Lim;Park, Jong-Sei
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.659-666
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    • 1991
  • A systematic analysis of 18 stimulants and narcotic analgesics containing nitrogen atom (s) in human urine by gas chromatography with nitrogen phosphorus detector (GC-NPD), is described. The urinary extract with diethyl ether at pH 8.5 showed good recoveries of the drugs and less interference peaks on GC chromatogram. Retention data were standardized by the calculation of relative retention times using diphenylamine as the internal standard. The relative standard deviations of retention times were less than 0.1% for the within-run analyses. The response factor (RRF) of a drug relative to the internal standard was calculated. RRF decreased with increasing number of nitrogen atoms. This technique can be adapted to various analytical toxicology problems.

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