Research has centred on multidimensional chromatographic techniques which utilise the high specificity of immunoaffinity chromatography for extraction of analytes from complex biological matrices. On-line immunoaffinity chromatography-high performance liquid chromatography-mass spectrometry (IAC-HPLC-MS) systems (IAC and HPLC coupled via a loop interface) were developed for the confirmatory analysis of the corticosteroids dexamethasone and flumethasone with MS detection. Utilising an atmospheric pressure chemical ionisation (APCI) LC-MS interface, dexamethasone was confirmed in both spiked and post administration equine urine samples, with a detection limit of 0.1 ug 1-l. Detection by quadrupole ion trap mass spectrometry (ITMS) using a particle beam (PB) interface was performed for dexamethasone and flumethasone in post administration equine urine samples with high precision (6.9-7.4 %) with limits of detection in the range 3-4 ug 1-l. Studies were also conducted in this work into the antibody crossreactivity and non-specific binding of corticosteroids on a HEMA bound anti-dexamethasone lAC column. On-line IAC-HPLC and IAC-HPLC-GC have been developed and assessed for the determination of testosterone in equine urine. A novel approach to interfacing lAC with HPLC being achieved using a porous graphitic carbon (PGC) column. The IAC-HPLC system developed was used for sample pre-treatment for combustion isotope ratio mass spectrometry analysis. The IAC-HPLC and IAC-HPLC-GC systems finally being coupled with mass spectrometry to enable confirmation of the endogenous steroid at 0.5 ug 1-l and 1 ug 1-l respectively in stripped equine urine.
| Identifer | oai:union.ndltd.org:bl.uk/oai:ethos.bl.uk:388946 |
| Date | January 1997 |
| Creators | Feely, Stephen Joseph |
| Publisher | Nottingham Trent University |
| Source Sets | Ethos UK |
| Detected Language | English |
| Type | Electronic Thesis or Dissertation |
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