title: Fully automated analytical system using liquid-solid extraction and liquid chromatography for the determination of CGP 6140 in plasma.
abstract: Liquid-solid extraction on disposable extraction columns (DECs) and liquid chromatography can be combined in a completely automated analyser. The Gilson ASPEC system was used to develop a procedure for the determination of CGP 6140 in plasma. Both sample preparation via C8 Bond-Elut DECs and injection were fully automatic. The fully automated system prepared the samples by performing the same operations as for a manual procedure. The DEC was first wetted with methanol, then with water. A 400-microliters volume of plasma and 40 microliters of the internal standard solution, diluted with 1 ml of water, were applied to the DEC, rinsed with 10(-2) mol/l dipotassium hydrogenphosphate and eluted from the DEC with 300 microliters of acetonitrile-methanol (50:50, v/v). The eluting strength of the eluate was reduced by dispensing 1 ml of water into each vial prior to direct injection into a Spherisorb ODS column via a 1-ml loop. This allowed the reconcentration of the extracted compounds on the top of the column, as they were injected in a large volume of solvent of lower eluting strength than the mobile phase [acetonitrile-methanol-4 x 10(-3) mol/l ammonia solution (54.5:5:40.5, v/v/v)]. Reproducibility results are presented.
authors.affiliation: Laboratoires Ciba-Geigy, Biopharmaceutical Research Centre, Rueil-Malmaison, France.
authors.forename: M C
authors.initials: MC
authors.lastname: Rouan
authors.forename: J
authors.initials: J
authors.lastname: Campestrini
authors.forename: J B
authors.initials: JB
authors.lastname: Lecaillon
authors.forename: J P
authors.initials: JP
authors.lastname: Dubois
authors.forename: M
authors.initials: M
authors.lastname: Lamontagne
authors.forename: B
authors.initials: B
authors.lastname: Pichon
mesh_terms: D055598:Chemical Phenomena; D002621:Chemistry; D002853:Chromatography, Liquid / Q000295:instrumentation; D006801:Humans; D010879:Piperazines / Q000097:blood*
chemical_list: D010879:Piperazines; C051744:amocarzine