The objectives of these studies was to investigate the use of tris(2,4,6-trimethoxyphenyl) phosphonium (TMPP) derivatising reagents to enhance methods for the analysis of acids, alcohols and amines by high-performance liquid chromatography-mass spectrometry (LC-MS). Early chapters provide an introduction to the main instrumental techniques of chromatography, mass spectrometry and solid phase extraction used to conduct the experiments in the thesis. This is followed by a review of derivatisation for compounds analysed with HPLC and LC-MS. Particular emphasis is placed on tris(2,4,6-trimethoxyphenyl) phosphonium reagents. Chapter three provides experimental and instrumental details together with descriptions of the synthesis of the TMPP derivatising reagents. LC-MS studies on underivatised and derivatised compounds were conducted using electrospray ionisation (ESI) and atmospheric pressure chemical ionisation (APCI) with the positive ionisation mode providing to be the method of choice for derivatised compounds. Studies of carboxylic acids showed that derivatives formed with tris(2,4,6-trimethoyphenyl)phosphonum propylamine (TMPPPrNH<sub>2</sub>) gave lower detection limits by LC-MS. The technique was successfully applied to the qualitative and quantitative analysis of the fatty acids composition of a variety of cooking oils and to the analysis of the fatty acids in soil extracts. Similar enhancement in sensitivity for LC-MS by ESI and APCI was observed for the TMPP derivatives of phenoxyalkanoic acid (PAAs) herbicides. Spiked water samples were studied using solid phase extraction and derivatisation of the herbicides were detected at low ng/L levels. Encouraged by these studies bile acids were next investigated and derivatisation of the carboxylic acid group with TMPPPrNH<sub>2</sub> provided enhanced sensitivity for LC-MS. The technique was successfully applied to the analysis of bovine bile for bile acids but taurine conjugated acids were not detected. TMPP derivatives provide improved methods for the analysis of acids, alcohols and amines by LC-MS using either ESI or APCI.
| Identifer | oai:union.ndltd.org:bl.uk/oai:ethos.bl.uk:638767 |
| Date | January 2005 |
| Creators | Sangsrichan, S. |
| Publisher | Swansea University |
| Source Sets | Ethos UK |
| Detected Language | English |
| Type | Electronic Thesis or Dissertation |
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