• 제목/요약/키워드: Doping control analysis

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Simultaneous Liquid Chromatography Tandem Mass Spectrometric Determination of 35 Prohibited Substances in Equine Plasma for Doping Control

  • Kwak, Young Beom;Yu, Jundong;Yoo, Hye Hyun
    • Mass Spectrometry Letters
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    • 제13권4호
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    • pp.158-165
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    • 2022
  • Many therapeutic class drugs such as beta-blocker, corticosteroids, NSAIDs, etc are prohibited substances in the horse racing industry. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology makes it possible to isolate drugs from interference, enables various drug analyses in complex biological samples due to its sensitive sensitivity, and has been successfully applied to doping control. In this paper, we describe a rapid and sensitive method based on solid-phase extraction (SPE) using solid phase cartridge and LC-MS/MS to screen for different class's 35 drug targets in equine plasma. Plasma samples were pretreated by SPE with the NEXUS cartridge consisted non-polar carbon resin and minimum buffer solvent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 ㎛). The elution gradient was conducted with 5 mM ammonium formate (pH 3.0) in distilled water and 0.1% formic acid in acetonitrile at a flow rate of 0.25 mL/min. The selected reaction monitoring (SRM) mode was used for drug screening with multiple transitions in the positive ionization mode. The specificity, limit of detection, recovery, and stability was evaluated for validation. The method was found to be sensitive and reproducible for drug screening. The method was applied to plasma sample analysis for the proficiency test from the Association of Racing Chemist.

Solution Dynamics Studies for the Lck SH2 Domain Complexed with Peptide and Peptide-Free Forms

  • Yoon, Jeong-Hyeok;Chi, Myung-Whan;Yoon, Chang-No;Park, Jongsei
    • 한국응용약물학회:학술대회논문집
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    • 한국응용약물학회 1995년도 춘계학술대회
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    • pp.81-81
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    • 1995
  • It is well known that Src Homology 2(SH2) domain in many intracellular signal transduction proteins is very important. The domain has about 100 amino acid residues and bind phosphotyrosine-containing peptide with high affinity and specificity. Lck SH2 domain is a Src-like, lymphocyte-specific tyrosine kinase. An 11-residue phosphopeptide derived from the hamster polvoma middle-T antigen, EPQp YEEIPIYL, binds with an 1 nM dissociation constant to Lck SH2 domain. And it is known that the phosphotyrosine and isoleucine residues of the peptide are tightly bound by two well-defined pockets on Lck SH2 domain's surface. To investigate the conformational changes during complexation of SH2 domain with phosphopeptide we have performed the molecular dynamics simulation for Lck SH2 domain with peptide and peptide-free form at look in aqueous solution. More than 3000 water molecules were incorporated to solvate Lck SH2 domain and peptide. Periodic boundary condition has been applied in molecular dynamics simulation. Data analysis with the results of that simulation shows that the phosphopeptide makes primary interaction with the Lck SH2 domain at six central residues, The comparison of the complexed and uncomplexed SH2 domain structures in solution has revealed only relatively small change. But the hydrophilic and hydrophobic pockets in the protein surface show the conformational changes in spite of the small structural difference between the complex and peptide-free forms.

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모작업장에서 휘발성 유기오염물질의 분석과 근로자들의 건강위해성 평가 (Health Risk Assessment and Analysis on the Volatile Organic Compounds in Some Workplace)

  • 이효민;김명수;최시내;윤은경;박종세
    • Journal of Preventive Medicine and Public Health
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    • 제30권3호
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    • pp.530-539
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    • 1997
  • This study was conducted to assess the health risk on the volatile organic compounds such as toluene, xylene, and styrene in painting workplace. It was monitored through personal air sampling during working time in selected 5 workplaces and analysed using gas chromatography. For the settlement of exposure situation, there were regarded working conditions such as working hours, yearly working days, and working years. Also, Monte-Carlo simulation was used for the induction of hazard index using toxicity value from IRIS(Integrated risk information system) database. The results of risk assessment were summarized as follows. 1. The air concentration of toluene was $7.096{\pm}15,644ppm,\;2.586{\pm}4.275ppm\;for\;xylene,\;1.914{\pm}5.320ppm$ for styrene in blast painting workplaces. The level of toluene was different significantly compared with the level of xylene and styrene. 2. Computated chronic daily intake values of 95th percentile on toluene, xylene and styrene treated by Monte-Carlo simulation were 9.616, 3.567, 2.782 mg/kg/day, respectively. 3. Computated hazard index values of 75th percentile on toluene, xylene and styrene treated by Monte-Carlo simulation were 3.5, 1.0 and 1.6, respectively. Adverse health effects on the toluene, xylene and styrene would be expected by working exposure in selected 5 workplaces since the hazard indices of three compounds were exceeded 1 in the surroundings of 75th percentile though having the low emerged frequency.

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운동선수들의 혈액분석을 통한 Etrythropoietin 간접도핑검사 (Blood Analysis for Indirect Doping Control of Erythropoietin in Sports)

  • 이정란;김소영;홍지연;김명수;최명자
    • 약학회지
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    • 제47권6호
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    • pp.422-431
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    • 2003
  • The use of recombinant human erythropoietin (rhEPO), a stimulator of erythropoiesis, banned in sports because of the medical risk associated with thrombosis. Due to analytical difficulties to differentiate between natural human EPO (hEPO) and rhEPO, blood parameters of erythropoiesis such as contents of hemoglobin (cut-off value <17.5 g/d l for man, and < 16.0 g/dl for women), hematocrit and reticulocytes (cut-off value <2.0%) were measured to focus the misuse of rhEPO. We conducted anti-doping test for 122 blood samples of the World Cup athletes. The mean values of key parameters are as follows; 14.5$\pm$1.0 g/dl for hemoglobin, 41.7$\pm$2.8% for hematocrit, and 1.3$\pm$0.4% for reticulocyte. Blood sample was found to be stable up to 8 hours for the reticulocyte measurement. In addition, the soluble transferrin receptor and ferritin levels were measured by immunoassay methods using plasma samples (n=28) in which the mean value was 0.8$\pm$0.5 $\mu\textrm{g}$/$m\ell$ and 54.6$\pm$33.7 ng/$m\ell$, respectively. The results indicate that all samples tested were negative for the blood parameters of indirect anti-doping test for hEPO misuse. The statistical evaluation suggest that several other parameters such as red blood cell, mean corpuscular hemoglobin concentration, mean corpuscular volume, mean corpuscular hemoglobin and white blood cell could be considered as factors influencing hEPO function in addition to five parameters mentioned.

Alternative Sample Preparation Techniques in Gas Chromatographic-Mass Spectrometric Analysis of Urinary Androgenic Steroids

  • Cho, Young-Dae;Choi, Man-Ho
    • Bulletin of the Korean Chemical Society
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    • 제27권9호
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    • pp.1315-1322
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    • 2006
  • The following study describes the gas chromatography-mass spectrometry (GC-MS) based screening and confirmation analysis of urinary androgenic steroids. Four commercially available solid-phase extraction (SPE) cartridges, Serdolit PAD-1, Sep-pak $C_{18}$, amino-propyl, and Oasis HLB, and three different extractive organic solvents, diethyl ether, methyl tert-butyl ether (MTBE), and n-pentane, were tested for sample preparation. Overall, Oasis HLB combined with MTBE extraction provided the highest recoveries in 39 of 46 total androgenic steroids examined and it showed a good extraction yield (>82.1%) for polar steroids, such as metabolites of fluoxymesterone, oxandrolone, and stanozolol, which gave a poor recovery in both n-pentane (9.2-64.3%) and diethyl ether (22.2-73.6%) extractions. All SPE sorbents tested showed potential, because they were efficient in extraction for most or selective steroids. When applied to positive urine samples based on the results obtained, the present method allowed selective and sensitive analysis for detection of urinary androgenic steroids. The experiments showed that the high-resolution MS method is clearly more efficient than the low-resolution MS technique for the detection of many urinary steroids. However, comprehensive sample clean-up procedures also might be needed especially in confirmation analysis to increase detectability.

Structural Analysis of the Ectodomain of HIV Gp41 and Implication on the Gp41 Assisted Membrane Fusion

  • Ryu, Jae-Ryen;Lee, Jung;Suh, Mu-Jin;Yu, Yeong-Sook;Yu, Yeon-Gyu
    • 한국생물물리학회:학술대회논문집
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    • 한국생물물리학회 1996년도 정기총회 및 학술발표회
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    • pp.33-33
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    • 1996
  • An ectodomain of gp41, the transmembrane fusion protein of HIV, without the fusion peptide region was expressed using pET system in E. coli. The expressed protein gp41core, was isolated as inclusion body and was purified by ion-exchange chromatography after solubilized in 6M urea. The purified denatured protein was renaturated and the folded domain of gp41core was identified by the presence of the proteolysis resistence domain and a high content of ${\alpha}$-helical secondary structure. (omitted)

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단일 Floating Island 구조 Power MOSFET의 전기적 특성 향상과 설계 파라미터에 관한 연구 (A Study on Electrical Characteristic Improvement & Design Parameters of Power MOSFET with Single Floating Island Structure)

  • 조유습;성만영
    • 한국전기전자재료학회논문지
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    • 제28권4호
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    • pp.222-228
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    • 2015
  • Power MOSFETs (metal oxide semiconductor field effect transistor) operate as energy control semiconductor switches. In order to reduce energy loss of the device, it is essential to increase its conductance. However, a trade-off relationship between the breakdown voltage and conductance of the device have been the critical difficulty to improve. In this paper, theoretical analysis of electrical benefits on single floating island power MOSFET is proposed. By the method, the optimization point has set defining the doping limit under single floating island structure. The numerical multiple 2.22 was obtained which indicates the doping limit of the original device, improving its ON state voltage drop by 45%.

HPLC 및 GC/MSD를 이용한 식물 중의 Higenamine 함량 분석 (Analysis of Higenamine Contents in Plants with HPLC and GC/MSD)

  • 윤혜숙;서영배;한영희;송윤선;류재천;정교순
    • 생약학회지
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    • 제29권2호
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    • pp.129-135
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    • 1998
  • Higenamine is known as a cardiotonic principle of Aconiti tuber. The analytical procedures were established for the detection of higenamine in plants. The amounts of higenamine in several Aconiti tubers and the embryo of Nelumbo nucifera, another plant species known to contain higenamine, were determined. The $H_2O$ soluble fraction prepared from MeOH extract was first treated with AD-2 resin and then applied to either HPLC or GC/MSD systems. With HPLC, $6.4{\sim}19.2\;{\mu}g/g$ of higenamine were detected from various Aconiti tubers and $182.3\;{\mu}g/g$ of higenamine from the embryo of Nelumbo nucifera. The results obtained with GC/MSD also provided comparable data with those obtained with HPLC.

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국가 바이오모니터링 프로그램을 위한 소변 중 금속류 동시분석법 개발 및 검증 (Development and Validation of the Simultaneous Analytical Method of Urinary Metals and Metalloids for the National Biomonitoring Programs)

  • 조용민;양민호;임호섭;차상원;이재익;김기훈;한상범
    • 한국환경보건학회지
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    • 제45권6호
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    • pp.594-604
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    • 2019
  • Objectives: This study developed and validated an analysis method of urinary metals and metalloids that can be applied inductively with coupled plasma mass spectrometry (ICP-MS). Methods: 0.3 mL of urine was used to analyze 25 metal and metalloid compounds using ICP-MS. The validation of the analytical method included linearity, accuracy, precision, and the calculation of detection limits. In addition, a comparison test was performed with the graphite furnace atomic absorption spectrometry (GF-AAS) method, which is the current standard method, with urine samples of 66 healthy subjects. Results: The linearities (R2) of calibration curves of all 25 compounds were ≥ 0.999. Of the 25 compounds, the intra-day and inter-day accuracy% of 17 and 20 met ≤15%, respectively. In addition, fifteen compounds showed ≤15% recovery% for certificated reference materials. Intraclass correlation coefficients of the comparison between the current methods and new methods in this study were 0.952 (p-value<0.001) and 0.911 (p-value<0.001) for urinary cadmium and mercury, respectively. Conclusion: This study proposes an efficient simultaneous methodology that can analyze multi elements in smaller sample amounts. More reproduction experiments are needed in the future.

이차원 양자 효과를 고려한 극미세 Double-Gate MOSFET (2D Quantum Effect Analysis of Nanoscale Double-Gate MOSFET)

  • 김지현;손애리;정나래;신형순
    • 대한전자공학회논문지SD
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    • 제45권10호
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    • pp.15-22
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    • 2008
  • 기존의 MOSFET는 단채널 현상의 증가로 인하여 스케일링에 한계를 가지고 있다. Double-Gate MOSFET (DG-MOSFET)는 소자의 길이가 축소되면서 나타나는 단채널 현상을 효과적으로 제어하는 차세대 소자이다. DG-MOSFET으로 소자를 축소시키면 채널 길이가 10nm 이하에서 게이트 방향뿐만 아니라 소스와 드레인 방향에서도 양자 효과가 발생한다. 또한 게이트 길이가 매우 짧아지면 ballistic transport 현상이 발생한다. 따라서 본 연구에서는 2차원 양자 효과와 ballistic transport를 고려하여 DG-MOSFET의 특성을 분석하였다. 또한 단채널 효과를 줄이기 위해서 $t_{si}$와 underlap 그리고 lateral doping gradient를 이용하여 소자 구조를 최적화하였다.