Detection of multiple steroidal compounds in synthetic urine using comprehensive gas chromatography-mass spectrometry (GC×GC-MS) combined with a molecularly imprinted polymer clean-up protocol

Analyst Pub Date: 2014-07-17 DOI: 10.1039/C4AN00721B

Abstract

A method capable of screening for multiple steroids in urine has been developed, using a series of twelve structurally similar, and commercially relevant compounds as target analytes. A molecularly imprinted solid phase extraction clean-up step was used to make the sample suitable for injection onto a GC×GC-MS setup. Significant improvements compared to a commercially available C-18 material were observed. Each individual steroid was able to be separated and identified, using both the retention profile and diagnostic fragmentation ion monitoring abilities of the comprehensive chromatographic-mass spectrometry method. Effective LODs of between 11.7 and 27.0 pg were calculated for individual steroids, effectively equivalent to concentration levels of between 0.234 and 0.540 ng mL?1 in urine, while the application of multiple screen was demonstrated using a 10 ng mL?1 mixed sample. The nature of this study also removes the need for sample derivitisation which speeds up the screening process.

Graphical abstract: Detection of multiple steroidal compounds in synthetic urine using comprehensive gas chromatography-mass spectrometry (GC×GC-MS) combined with a molecularly imprinted polymer clean-up protocol
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