title: Validation of a simple, sensitive method for the determination of beta-estradiol in bovine urine using gas-chromatography negative-ion chemical ionization mass spectrometry.
abstract: A new method is presented for the analysis of 17[small beta]-estradiol in bovine urine. After deconjugation, the sample is cleaned up using an OASIS[trade mark sign] HLB disposable cartridge and extracted into 1-chlorobutane. The hormone is derivatized using pentafluorobenzoyl chloride. The derivatized estradiol is quantitated using gas-chromatography negative-ion chemical ionization mass spectrometry. Calibrations, obtained using spiked blank urine, are linear in the range of 100-1000 pg mL(-1) with CC[small alpha] approximately 170 pg mL(-1) and CC[small beta] of 287 pg mL(-1). Recoveries are in the range of 80 to 130%. The method is rugged, rapid and sensitive when compared to other hormone methods.
authors.affiliation: Canadian Food Inspection Agency, Saskatoon Laboratory, Centre for Veterinary Drug Residues, 116 Veterinary Road, Saskatoon, SK, CanadaS7N 2R3. akrec@inspection.gc.ca
authors.forename: Christine
authors.initials: C
authors.lastname: Akre
authors.forename: Rick
authors.initials: R
authors.lastname: Fedeniuk
authors.forename: James D
authors.initials: JD
authors.lastname: MacNeil
mesh_terms: D000818:Animals; D002417:Cattle / Q000652:urine*; D004350:Drug Residues / Q000032:analysis*; D004958:Estradiol / Q000652:urine*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods / Q000662:veterinary
chemical_list: D004958:Estradiol