title: 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.
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.
authors.affiliation: Department of Physical Sciences, The Open University, Milton Keynes, MK7 6AA, UK.
authors.forename: Adnan
authors.initials: A
authors.lastname: Zulfiqar
authors.forename: Geraint
authors.initials: G
authors.lastname: Morgan
authors.forename: Nicholas W
authors.initials: NW
authors.lastname: Turner
mesh_terms: D002138:Calibration; D008401:Gas Chromatography-Mass Spectrometry / Q000592:standards; D006801:Humans; D007091:Image Processing, Computer-Assisted; D021621:Imaging, Three-Dimensional; D054802:Molecular Imprinting; D011108:Polymers / Q000737:chemistry; D052616:Solid Phase Extraction; D013256:Steroids / Q000032:analysis* / Q000302:isolation & purification / Q000652:urine
chemical_list: D011108:Polymers; D013256:Steroids