Validation of a simple method for the analysis of
Estradiol in bovine urine using gas-chromatography negative-ion chemical ionization mass spectrometry

C. Akre, R. Fedeniuk, J. MacNeil
Canadian Food Inspection Agency, Saskatoon Laboratory, Centre for Veterinary Drug Residues
116 Veterinary Road, Saskatoon, SK S7N 2R3, Canada.

Abstract

A new method is presented for the analysis of 17 -estradiol in bovine urine. After deconjugation, the sample is passed through an OASIS™ disposable cartridge and extracted into 1-chlorobutane. The hormones are 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 with limit of quantitation set at approximately 100 pg/mL. Stages of the validation procedure along with ruggedness testing of the procedure will be presented.