Fully automated analytical system using liquid-solid extraction and liquid chromatography for the determination of CGP 6140 in plasma.
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.
Rouan
M C
MC
Laboratoires Ciba-Geigy, Biopharmaceutical Research Centre, Rueil-Malmaison, France.
Campestrini
J
J
Lecaillon
J B
JB
Dubois
J P
JP
Lamontagne
M
M
Pichon
B
B
D055598:Chemical Phenomena; D002621:Chemistry; D002853:Chromatography, Liquid / Q000295:instrumentation; D006801:Humans; D010879:Piperazines / Q000097:blood*
D010879:Piperazines; C051744:amocarzine