Determination of Ketosteroids in Human Urine Using Dispersive Liquid-Liquid Microextraction and Ultra High-Performance Liquid Chromatography-High Resolution Mass Spectrometry

Abstract A method is proposed for the determination of some ketosteroids in human urine, including enzymatic hydrolysis using β-glucuronidase from E. coli followed by dispersive liquid-liquid microextraction, derivatization analytes with hydroxylamine, and detection reversed-phase ultra-HPLC–quadrupole time-of-flight mass spectrometry. Optimization extraction conditions studied compounds made it possible to find that highest recoveries were achieved an acetone–chloroform mixture as a dispersant extractant, completeness reaction was thermostating sample at 70°C 90 min. The has high sensitivity (limits range 0.1–0.25 ng/mL) wide linearity range.