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The chromatographic behaviour of four organophosphorus pesticides has been investigated, using capillary gas liquid chromatography-mass spectrometry (GC-MS), and packed and wide bore capillary gas liquid chromatography with electron capture detection (GC-ECD). The first part of this thesis (Chapter 3) embodies the application of high performance capillary gas liquid chromatography-mass spectrometry and the development of the methodology for analysis of pesticides in fruit and vegetable substrates. Manipulation of GC-MS data during the sample analysis is necessary in order to eliminate the problems arising from the complexity of the samples. The application of selected ion monitoring (SIM) in GC-MS is to a large extent limited by selection of the ion for monitoring, selection of internal standard, optimisation of electrometer zero, the electron multiplier voltage, the selected mass interval, column selection for GC-MS analysis and tuning of the quadrupole GC-MS. A major concern was with the determination of the optimum conditions for the analysis of substrates containing organophosphorus pesticides by GC-MS following solvent extraction (without clean up steps). The analysis of organophosphorus samples using GC-MS-SIM provides detection limits lower than Pg pesticide injected and very good recovery data. The second part (Chapter 4) deals with the application of GC-ECD. Here the role of packed column support, packed and wide bore capillary column temperature and detector temperature was investigated. Comparisons of the relative responses of the pesticides analysed (i) on packed columns and (ii) on wide bore capillary column under different column and detector cell temperatures were undertaken and the optimal condition for each of the organophosphorus pesticides was determined, under the optimal conditions the detection limits and recovery for fruit and vegetable samples were examined. The results from this method were correlated with the data obtained by GC-MS and found to be in very good agreement. The data obtained from analysis using GC-ECD was found to have a higher precision than that obtained by GC-MS, however GC-MS exhibited a higher selectivity for the determination of these pesticides.

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