title: Liquid chromatography-electrospray tandem mass spectrometric assay suitable for quantitation of halofuginone in plasma.
abstract: An LC-MS/MS method was developed to quantitate the potential antitumor agent halofuginone in plasma. The assay uses 0.2 ml of plasma; chlorohalofuginone internal standard; acetonitrile for protein precipitation; a Phenomenex SYNERGI 4 micro Polar RP 80A (4 microm, 100 mm x 2 mm) column; an isocratic mobile phase of methanol:water:formic acid (80:20:0.02, v/v/v); and positive-ion electrospray ionization with selective reaction monitoring detection. Halofuginone eluted at approximately 2.4 min, internal standard eluted at approximately 2.9 min, and no endogenous materials interfered with their measurement. The assay was accurate, precise, and linear between 0.1 and 100 ng/ml. Halofuginone could be quantitated in dog plasma for at least 24 h after an i.v. dose of 0.1mg/kg. The assay is being used in ongoing pharmacokinetic studies of halofuginone.
authors.affiliation: Molecular Therapeutics/Drug Discovery Program, University of Pittsburgh Cancer Institute, Room G27e, Hillman Research Pavilion, 5117 Centre Avenue, Pittsburgh, PA 15213-1863, USA.
authors.forename: Robert A
authors.initials: RA
authors.lastname: Parise
authors.forename: Barney R
authors.initials: BR
authors.lastname: Sparrow
authors.forename: John W
authors.initials: JW
authors.lastname: Merrill
authors.forename: Irma M
authors.initials: IM
authors.lastname: Grossi
authors.forename: Joseph M
authors.initials: JM
authors.lastname: Covey
authors.forename: James O
authors.initials: JO
authors.lastname: Peggins
authors.forename: Merrill J
authors.initials: MJ
authors.lastname: Egorin
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid; D003049:Coccidiostats / Q000097:blood* / Q000493:pharmacokinetics; D004285:Dogs; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D008970:Molecular Weight; D010880:Piperidines; D011799:Quinazolines / Q000097:blood* / Q000493:pharmacokinetics; D052999:Quinazolinones; D012015:Reference Standards; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization
chemical_list: D003049:Coccidiostats; D007202:Indicators and Reagents; D010880:Piperidines; D011799:Quinazolines; D052999:Quinazolinones; C010176:halofuginone