title: Two-dimensional high-performance liquid chromatography at low ng/ml levels of the anti-proliferative agent B859-35 in serum with automated sample clean-up, solid-phase trapping and ultraviolet detection.
abstract: An automated non-chiral high-performance liquid chromatographic method is described for the determination of the new anti-proliferative agent B859-35 in serum. This method employs sample clean-up of 1 ml of biofluid by liquid-solid extraction with the AASP (Advanced Automatic Sample Preparation) system. First separation is achieved on a LiChrospher-60-RP-Select-B column. A fraction of this elute is then collected by solid-phase trapping. Thereafter, the final chromatogram is developed on a narrow-bore Hypers1-CPS column and quantified with ultraviolet detection at 230 nm. The limit of quantitation of the assay is 250 ng/ml. Linearity was proven in the range 0.25-100 ng/ml. Typical figures for precision at these concentrations are 7.4 and 3.3%, and for accuracy 8.0 and 1.3%, respectively. An application of this method to the study of pharmacokinetics of B859-35 in serum samples of cancer patients is given.
authors.affiliation: Byk Gulden Pharmaceuticals, Konstanz, Germany.
authors.forename: K
authors.initials: K
authors.lastname: Zech
authors.forename: R
authors.initials: R
authors.lastname: Herzog
mesh_terms: D000970:Antineoplastic Agents / Q000097:blood*; D002455:Cell Division / Q000187:drug effects; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004095:Dihydropyridines / Q000097:blood* / Q000494:pharmacology; D006801:Humans; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet
chemical_list: D000970:Antineoplastic Agents; D004095:Dihydropyridines; C054074:niguldipine