Trace analysis of progesterone and 21 progestins in milk by ultra-performance liquid chromatography coupled with high-field quadrupole-orbitrap high-resolution mass spectrometry

Abstract

A method for rapid screening and quantification of progesterone and progestins in milks by ultrahigh-performance liquid chromatography coupled with quadrupole-high field Orbitrap high-resolution mass spectrometry (UHPLC QE HF HRMS) was established. Milks samples were extracted by acetonitrile + hexane (80 + 20), purified by prime HLB SPE and analyzed by UHPLC QE HF HRMS. The detection limit of progesterone and 21 progestins in milk is between 0.05 µg/kg -0.3 μg /kg, the correlation coefficient of progesterone and progestins in the corresponding concentration range is more than 0.99, recoveries for milk samples are between 80.7% and 108.3% with the relative deviation is less than 15%.The method fulfils the requirements of veterinary drug residue detection validation of EU and China, and successfully applied to detecting the μg/kg level of progesterone and monitoring residual of progestins in real milk.

Keywords: High-performance liquid chromatography quadrupole-Orbitrap high-resolution mass spectrometry; Milk; Progesterone; Progestins.