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고체상추출 및 초고성능액체크로마토그래피-큐오비트랩질량분석기를 이용한 사람 소변 중 암페타민류 스크리닝
유준동(Jundong Yu),윤혜란(Hye-Ran Yoon) 대한약학회 2021 약학회지 Vol.65 No.6
We developed and validated a simple, sensitive, and reproducible analytical method using ultra high-pressure liquid chromatography (UHPLC)-QOrbitrap mass spectrometry to screen human urine samples for amphetamines. Amphetamines are classified under the group of abused drugs and are frequently used by jockeys. A rapid analysis method is necessary to ascertain the presence of minimal amounts of prohibited amphetamines in the urine samples of jockeys on a race day. For the method described herein, UHPLC conditions were set with a Luna Omega?? C18 column using a gradient mobile phase. Six amphetamines were separated by gradient elution and detected by QOrbitrap MS in the positive ion mode. Validation parameters, including selectivity and limit of detection, were evaluated for the purpose of screening for amphetamines in human urine. Human urine samples were prepared for analysis using enzymatic hydrolysis and solidphase extraction. The limit of detection for screening the six amphetamines was between 0.1-10 ng/mL. We obtained recoveries between 31% and 76%, which is suitable for screening the amphetamines. This method combines the advantages of SPE and UHPLC-QOrbitrap MS, such as an effective extraction and simple analysis steps, and validated the amphetamine screening method for drug abuse control of jockies and improving public health.
Young Beom Kwak,Jundong Yu,Hye Hyun Yoo 사단법인 한국질량분석학회 2022 Mass spectrometry letters Vol.13 No.4
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 sol- vent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 µm). 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.