title: Simple method for determination of triazolam in human plasma by high-performance liquid chromatography/tandem mass spectrometry.
abstract: Triazolam was analyzed from human plasma samples by high-performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) with an MSpak GF polymer column (50 mm x 4.6 mm i.d., particle size 6 microm), which enabled direct injection of crude biological samples. Separation of triazolam, and lorazepam as the internal standard (IS) was carried out using 10mM ammonium acetate (pH 3.56)-0.1% formic acid and an acetonitrile gradient elution. Both compounds formed base peaks due to [M + H]+ ions by HPLC/ESI-MS, and product ions were produced from each [M + H]+ ion as seen by HPLC-MS/MS. Quantification of triazolam and the IS in plasma samples was made by selective reaction monitoring using each base peak of product ions of HPLC-MS/MS. The recovery range of triazolam spiked into plasma was 86.4-92.7%. The regression equation for triazolam showed excellent linearity in the range of 0.25-20 ng/mL, and the detection limit was 0.1 ng/mL. Intra- and inter-day precisions for triazolam in plasma samples were not greater than 12.4%. Accuracy for the drug was in the range of 88.0-101.4%. Data obtained after oral administration of triazolam in male and female subjects are also presented.
authors.affiliation: Department of Legal Medicine, Showa University School of Medicine, 1-5-8 Hatanodai, Shinagawa-ku, Tokyo 142-8555, Japan.
authors.forename: Xiao-Pen
authors.initials: XP
authors.lastname: Lee
authors.forename: Takeshi
authors.initials: T
authors.lastname: Kumazawa
authors.forename: Masaya
authors.initials: M
authors.lastname: Fujishiro
authors.forename: Chika
authors.initials: C
authors.lastname: Hasegawa
authors.forename: Akemi
authors.initials: A
authors.lastname: Marumo
authors.forename: Yukiko
authors.initials: Y
authors.lastname: Shoji
authors.forename: Tetsuya
authors.initials: T
authors.lastname: Arinobu
authors.forename: Hiroshi
authors.initials: H
authors.lastname: Seno
authors.forename: Keizo
authors.initials: K
authors.lastname: Sato
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D000284:Administration, Oral; D000328:Adult; D002626:Chemistry, Pharmaceutical / Q000379:methods; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005260:Female; D005561:Formates / Q000737:chemistry; D006801:Humans; D006863:Hydrogen-Ion Concentration; D008297:Male; D013058:Mass Spectrometry / Q000379:methods*; D008956:Models, Chemical; D012044:Regression Analysis; D015203:Reproducibility of Results; D014229:Triazolam / Q000032:analysis* / Q000097:blood*
chemical_list: D000097:Acetonitriles; D005561:Formates; C030544:formic acid; D014229:Triazolam; C032159:acetonitrile