title: Determination of diastereoisomers of bromadiolone, an anticoagulant rodenticide, in animal tissues by high-performance liquid chromatography.
abstract: Two components isolated by semi-preparative normal phase high-performance liquid chromatography (HPLC) of bromadiolone reference material were tentatively identified as diastereoisomeric forms. Examination by mass spectroscopy confirmed this identification and supporting evidence was provided by identical UV fluorescence characteristics. The separated isomers were used to examine the chromatographic properties of bromadiolone in ion-pair, ion-suppression and weak ion-exchange HPLC modes. Conditions suitable for the analytical determination of the individual diastereoisomers were established for each mode. The influence of mobile phase pH on the resolution of coumarin-based rodenticides by weak ion-exchange HPLC on an aminopropyl-bonded phase was studied. Clean-up techniques for the determination of residues of bromadiolone in animal tissue extracts were compared. A combined gel permeation and adsorption chromatographic procedure was preferred for sensitive assay; it permitted the use of either fluorescence or UV detection. The lower practical limit of determination of each isomer in animal tissues was 0.005 mg kg-1 using UV detection and 0.0005 mg kg-1 using fluorescence detection.
authors.affiliation: Department of Agriculture and Fisheries for Scotland, Agricultural Scientific Services, East Craigs, Edinburgh, U.K.
authors.forename: K
authors.initials: K
authors.lastname: Hunter
authors.forename: E A
authors.initials: EA
authors.lastname: Sharp
authors.forename: A
authors.initials: A
authors.lastname: Newton
mesh_terms: D015110:4-Hydroxycoumarins / Q000032:analysis*; D000818:Animals; D002851:Chromatography, High Pressure Liquid; D002852:Chromatography, Ion Exchange; D004285:Dogs; D006863:Hydrogen-Ion Concentration; D008099:Liver / Q000032:analysis; D013058:Mass Spectrometry; D011817:Rabbits; D012378:Rodenticides / Q000032:analysis*; D013050:Spectrometry, Fluorescence; D013056:Spectrophotometry, Ultraviolet; D013237:Stereoisomerism
chemical_list: D015110:4-Hydroxycoumarins; D012378:Rodenticides; C021636:bromadiolone