title: Direct and rapid quantitation of ephedrines in human urine by paper spray ionization/high resolution mass spectrometry.
abstract: A rapid and direct paper spray ionization/mass spectrometry (PSI/MS) method was developed for quantitative analysis of ephedrine, pseudoephedrine, norpseudoephedrine, and methylephedrine in human urine. This method involves the use of a triangular filter paper and high-resolution mass spectrometry, where the molecular ions of ephedrines were generated by applying high voltage after loading the spray solvent to the paper which urine sample was pre-loaded. Small amounts (2μL) of urine spiked with an internal standard were directly analyzed for ephedrines. The PSI/MS method was validated for linearity, within- and between-run precision, accuracy, and limit of detection. The results showed good linearity (R(2)≥0.9928) and acceptable precision and accuracy. Furthermore, the accuracy of the method was assessed by analyzing a blind urine sample from World Anti-Doping Agency and comparing the measured concentrations with the nominal concentrations. This test resulted in accuracies ranging from 96.4 to 106.1%, indicating that the PSI/MS method has the potential to be an alternative technique for the fast quantitation of ephedrines in doping control analysis.
authors.affiliation: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Republic of Korea.
authors.forename: Eun Sook
authors.initials: ES
authors.lastname: Jeong
authors.affiliation: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Republic of Korea.
authors.forename: Ki Hun
authors.initials: KH
authors.lastname: Kim
authors.affiliation: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Republic of Korea.
authors.forename: Eunju
authors.initials: E
authors.lastname: Cha
authors.affiliation: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Republic of Korea.
authors.forename: Oh-Seung
authors.initials: OS
authors.lastname: Kwon
authors.affiliation: Department of Chemistry, Hankuk University of Foreign Studies, Yongin, 449-791, Republic of Korea.
authors.forename: Sangwon
authors.initials: S
authors.lastname: Cha
authors.affiliation: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Republic of Korea. Electronic address: jaeicklee@kist.re.kr.
authors.forename: Jaeick
authors.initials: J
authors.lastname: Lee
mesh_terms: D000697:Central Nervous System Stimulants / Q000652:urine*; D004809:Ephedrine / Q000031:analogs & derivatives* / Q000652:urine*; D006801:Humans; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000191:economics / Q000379:methods*; D010209:Paper; D010665:Phenylpropanolamine / Q000652:urine*; D054199:Pseudoephedrine / Q000652:urine*; D015203:Reproducibility of Results; D015813:Substance Abuse Detection / Q000191:economics / Q000379:methods*
chemical_list: D000697:Central Nervous System Stimulants; C005331:norpseudoephedrine; D010665:Phenylpropanolamine; C041707:N-methylephedrine; D054199:Pseudoephedrine; D004809:Ephedrine
keywords: Doping control analysis; Ephedrine; Paper spray ionization/mass spectrometry