title: Semi-automated 96-well solid-phase extraction and gas chromatography-negative chemical ionization tandem mass spectrometry for the trace analysis of fluprostenol in rat plasma.
abstract: Semi-automated 96-well plate solid-phase extraction (SPE) was used for sample preparation of fluprostenol, a prostaglandin analog, in rat plasma prior to detection by gas chromatography-negative chemical ionization tandem mass spectrometry (GC-NCI-MS-MS). A liquid handling system was utilized for all aspects of sample handling prior to SPE including transferring of samples into a 96-well format, preparation of standards as well as addition of internal standard to standards, quality control samples and study samples. SPE was performed in a 96-well plate format using octadecylsilane packing and the effluent from the SPE was dried in a custom-made 96-well apparatus. The sample residue was derivatized sequentially with pentafluorobenzylbromide followed by N-methyl-N-trimethylsilyltrifluoroacetamide. The derivatized sample was then analyzed using GC-NCI-MS-MS. The dynamic range for the method was from 7 to 5800 pg/ml with a 0.1-ml plasma sample. The methodology was evaluated over a 4-day period and demonstrated an accuracy of 90-106% with a precision of 2.4-12.9%.
authors.affiliation: Procter & Gamble Pharmaceuticals, Mason, OH 45040, USA.
authors.forename: R D
authors.initials: RD
authors.lastname: Gauw
authors.forename: P J
authors.initials: PJ
authors.lastname: Stoffolano
authors.forename: D L
authors.initials: DL
authors.lastname: Kuhlenbeck
authors.forename: V S
authors.initials: VS
authors.lastname: Patel
authors.forename: S M
authors.initials: SM
authors.lastname: Garver
authors.forename: T R
authors.initials: TR
authors.lastname: Baker
authors.forename: K R
authors.initials: KR
authors.lastname: Wehmeyer
mesh_terms: D000818:Animals; D002138:Calibration; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008297:Male; D011461:Prostaglandins F, Synthetic / Q000097:blood* / Q000493:pharmacokinetics; D051381:Rats; D017207:Rats, Sprague-Dawley; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D011461:Prostaglandins F, Synthetic; C006326:fluprostenol