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
Rd. Gauw et al., 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, J CHROMAT B, 744(2), 2000, pp. 283-291
Semi-automated 96-well plate solid-phase extraction (SPE) was used for samp
le preparation of fluprostenol, a prostaglandin analog, in rat plasma prior
to detection by gas chromatography-negative chemical ionization tandem mas
s spectrometry (GC-NCI-MS-MS). A liquid handling system was utilized for al
l aspects of sample handling prior to SPE including transferring of samples
into a 96-well format, preparation of standards as well as addition of int
ernal 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 sa
mple 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%. (C) 2000 Elsevier Science B.V. All rights reserve
d.