Validation of a simple, sensitive method for the determination of β-estradiol in bovine urine using gas-chromatography negative-ion chemical ionization mass spectrometry

Abstract

A new method is presented for the analysis of 17β-estradiol in bovine urine. After deconjugation, the sample is cleaned up using an OASIS™ 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 CCα approximately 170 pg mL⁻¹ and CCβ 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.