title: Determination of a major metabolite of tipredane in rat urine by high-performance liquid chromatography with column switching.
abstract: An automated method, based on column-switching reversed-phase high-performance liquid chromatography, has been developed for the determination of a major metabolite of tipredane in rat urine. Samples are injected directly onto a cyanopropyl extraction column. The portion of eluate containing the metabolite is switched, via an injection loop, onto an octadecylsilane analytical column. The limit of quantification of the method was 25 ng/ml for a 20 microl injection volume of urine. The intra-assay precision (0.7-4.8%) and accuracy (94-105%), and the inter-assay precision (2.7-12.6%) and accuracy (94-105%), were acceptable. The analyte was found to be stable in rat urine when stored at room temperature for six days, in a freezer at or below -20 degrees C for twelve weeks, and when the samples were subjected to two freeze-thaw cycles. No significant interference was observed from tipredane and its major human metabolites, or urine constituents in male and female rats. The method was successfully used to analyse samples from a long-term toxicology study.
authors.affiliation: Fisons plc, Research and Development Laboratories, Department of Physical Chemistry, Loughborough, Leicestershire, UK.
authors.forename: P R
authors.initials: PR
authors.lastname: Baker
authors.forename: M A
authors.initials: MA
authors.lastname: Bayliss
authors.forename: D
authors.initials: D
authors.lastname: Wilkinson
mesh_terms: D000287:Administration, Topical; D000730:Androstadienes / Q000378:metabolism* / Q000633:toxicity / Q000652:urine*; D000818:Animals; D000893:Anti-Inflammatory Agents / Q000378:metabolism* / Q000633:toxicity; D002851:Chromatography, High Pressure Liquid; D004355:Drug Stability; D005260:Female; D005938:Glucocorticoids; D008297:Male; D051381:Rats; D012680:Sensitivity and Specificity; D013450:Sulfones / Q000652:urine*; D013452:Sulfonium Compounds / Q000652:urine*
chemical_list: D000730:Androstadienes; D000893:Anti-Inflammatory Agents; D005938:Glucocorticoids; D013450:Sulfones; D013452:Sulfonium Compounds; C107421:FPL 66366XX; C107420:FPL 66365XX; C051756:tipredane; C107419:FPL 67336XX