Multidimensional chromatographic/mass spectrometric techniques for the trace determination of steroids.

Feely, S.J., 1997. Multidimensional chromatographic/mass spectrometric techniques for the trace determination of steroids. PhD, Nottingham Trent University.

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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 μg 1-1. 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 μg 1-1. Studies were also conducted in this work into the antibody crossreactivity and non-specific binding of corticosteroids on a HEMA bound anti-dexamethasone IAC 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 IAC 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 μg 1-1 and 1 μg 1-1 respectively in stripped equine urine.

Item Type: Thesis
Creators: Feely, S.J.
Date: 1997
ISBN: 9781369313093
Divisions: Schools > School of Animal, Rural and Environmental Sciences
Record created by: Jeremy Silvester
Date Added: 02 Sep 2020 09:36
Last Modified: 15 Jun 2023 10:05

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