Abstract: A simple, rapid and sensitive method for the simultaneous determination of 18 kinds of glucocorticoids in milk was developed by the quick, easy, cheap, effective, rugged and safe (QuEChERS) method coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) in the multiple reaction monitoring (MRM) mode. Milk samples were extracted with acidified acetonitrile, and salted out by adding sodium chloride anhydrous sodium magnesium sulfate. After purification with PSA and C18 as the adsorbent, the supernatant was analyzed by HPLC-MS/MS. The matrix effect in the method was in the range of 0.81–0.96, the limits of detection (LODs) were in the range of 0.1–0.3 μg/kg and the limits of quantification (LOQs) for the analytes were in range of 0.3–1.1 μg/kg. The method exhibited a good linear relationship in the range of 0.5–100 ng/mL, with a correlation coefficient (R2) of higher than 0.993 6, and recoveries were between 73.7% and 98.6% at three spiked levels with relative standard deviations (n = 5) of 4.9%–12.9%. This method was simple, accurate, reliable, and suitable for the rapid detection of glucocorticoids in bulk serum samples.

Key words: milk, QuEChERS, glucocorticoids, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)