A novel interface for the coupling of high performance liquid chromatography (HPLC) with
inductively coupled plasma mass spectrometry (ICP-MS) for the speciation of organometallic
compounds has been developed and utilised for a number of diverse applications.
Desolvation of the sample prior to reaching the plasma is shown to facilitate a more versatile
coupling of the two instrumental techniques. This has been achieved by first volatilising the
aerosol after nebulisation of the sample in a heated cyclone spray chamber. The resulting vapour
is removed using a membrane drier and a thermoelectrically cooled condenser. The apparatus
developed has been fully optimised to facilitate the introduction of a range of organic solvents,
particularly those used as mobile phases for HPLC separations such as acetonitrile and methanol.
This interface also facilitates gradient elutions to be used with ICP-MS for the first time.
The interface developed has enabled the use of HPLC-ICP-MS to speciate the metabolites of a
novel platinum based chemotherapy drug, JM-216, in human plasma ultrafiltrate. This approach
offers a number of advantages over existing techniques especially in terms of speed of analysis
and sensitivity. The platinum containing metabolites derived from this drug have been separated,
identified, and compared to those arising from the breakdown of cisplatin and carboplatin in both
plasma ultrafiltrate and an aqueous solution. A detection limit of 119 pg of Pt has been achieved
for real samples.
The interface has also been used for the speciation of organotin and organolead compounds in
environmental samples, and to investigate the speciation of metals in tea liquors. It was found
that although the apparatus proved beneficial for both the determination of organotins and the
identification of metal containing species in tea, its use adversely affected the analysis of
organolead compounds. The results of these latter studies are critically assessed and discussed
with respect to HPLC-ICP-MS interface design.
Date of Award | 1996 |
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Original language | English |
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Awarding Institution | |
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Interfacing High Performance Liquid Chromatography with Inductively Coupled Plasma Mass Spectrometry for Speciation Studies
Cairns, W. R. L. (Author). 1996
Student thesis: PhD