Extraction of glucocorticoids from water into acetonitrile using polyol induced extraction with ultra performance liquid chromatography and triple quadrupole mass spectrometry (PIE-UPLC-MS-MS)

Abstract

Polyol-induced Extraction (PIE) was used for the extraction and UPLC-MS-MS was used for the analysis of glucocorticoids in water. The focus of this work was to demonstrate PIE as an effective technique that allows extraction of solutes between miscible solutes using a phase separating agent, with an example analysis of glucocorticoids. In this work glycerol is used as the mass separating agent in the extraction of glucocorticoids from water into acetonitrile. Eight glucocorticoids were extracted by PIE and analyzed by UPLC-MS-MS. Extraction conditions were optimized, and extraction results were compared to non-extracted glucocorticoid standards and to literature methods. Extraction was optimized at 0 °C, in 10 mL of a 1:1 ACN/Water mixture 2 mL of glycerol added as phase separating agent. Calibration curves showed overall correlation of r² > 0.99. Precent relative standard deviation below 4%was obtained for all analytes. Limits of detection were obtained between 3–4 ng/mL by the IUPAC method and 40–200 ng/mL by a propagation of errors method. PIE is demonstrated to be a simple and quick method for extracting glucocorticoids from water into a miscible polar solvent, acetonitrile.

Graphical Abstract

Keywords:

• Glucocorticoids
• liquid chromatography
• PIE
• polyol induced extraction
• UPLC-MS-MS

Acknowledgements

NS gratefully acknowledges support for his endowed professorship from Thomas and Sylvia Tencza. Perkin Elmer is gratefully acknowledged for providing the UPLC-MS-MS system.