Validation of a simple, sensitive method for the determination of beta-estradiol in bovine urine using gas-chromatography negative-ion chemical ionization mass spectrometry |
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Authors: | Akre Christine Fedeniuk Rick MacNeil James D |
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Affiliation: | Canadian Food Inspection Agency, Saskatoon Laboratory, Centre for Veterinary Drug Residues, 116 Veterinary Road, Saskatoon, SK, CanadaS7N 2R3. akrec@inspection.gc.ca |
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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. |
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