Development an automated and high-throughput analytical platform for screening 39 glucocorticoids in animal-derived food for doping control

Abstract

For the purpose of doping control, increasing demand has been highlighted for the determination of glucocorticoids in animal derived foods. Although several methods have been established, the barrier of low throughput still exists for doping control. Herein, we report an on-line purification and high throughput platform for fast screening of 39 glucocorticoids in animal-derived food (pork, chicken, milk and eggs) using on-line solid-phase extraction (SPE) technology and liquid chromatography-tandem high-resolution mass spectrometry (LC-HRMS). An in-house developed, low-cost monolithic column was applied in this work which prevented the requirement of laborious and costly off-line solid-phase extraction columns. With one-step extraction and replacement of solvent, the sample can be directly and automatically injected as well as purified to screen 39 glucocorticoids in a single run time. The overall recoveries ranged from 62.0%–116.3% with intraday and inter-day relative standard deviation lower than 10.9% and 12.4%, respectively. The limits of quantitation for different matrices were between 0.84 and 4.94 μg/kg. Compared to the previous methods, the platform developed in this study shows excellent performance for rapid analysis of large numbers of samples and a wide variety of compounds with respect to short running time, analytical specificity and sensitivity as well as overall method accuracy and precision. In conclusion, this platform can function as a high-throughput tool in the field of doping analysis and contribute to a better safety assurance of animal-derived food.