Rapid determination of 18 glucocorticoids in serum using reusable on-line SPE polymeric monolithic column coupled with LC-quadrupole/orbitrap high-resolution mass spectrometer.

摘要: A simple, rapid and sensitive method for the simultaneous determination of 18 glucocorticoids in serum was developed by coupling on-line solid-phase extraction (SPE) polymeric monolithic column to a liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometer. simple poly(ethylene glycol dimethacrylate) monolith (10mm×2.1mm i.d.) fabricated, morphology, surface area performance were characterized. Serum samples extracted acetonitrile (ACN). Then, online SPE achieved on synthesized using 10mmol/L ammonium acetate solution as loading solvent. After transfer from into analytical (Capcell Pak ADME column) ACN, adsorbed analytes separated detected with hybrid quadrupole/orbitrap spectrometer full scan/ddMS2 scan mode Under optimized conditions, linear target correlation coefficient (R2) higher than 0.995. Detection limits range 0.1-0.6ng/mL, quantification 0.3-1.5ng/mL. The recovery between 71.9% 89.2% three spike levels precision (n=5) 5.40-12.1%. sample directly analyzed after procedure, within only 16min. used analyze dynamic contents variation cortisone hydrocortisone before surgery.