A post-column extraction system for the determination of tertiary amines by liquid chromatography with chemiluminescence detection |
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Authors: | P. J. M. Kwakman U. A. Th. Brinkman R. W. Frei G. J. de Jong F. J. Spruit N. G. F. M. Lammers J. H. M. van den Berg |
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Affiliation: | (1) Department of Analytical Chemistry, Free University, De Boelelaan 1083, 1081 HV Amsterdam, The Netherlands;(2) Duphar B.V., P. O. Box 2, 1380 AA Weesp, The Netherlands |
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Abstract: | Summary The combination of an ion-pair extraction detection system with peroxyoxalate chemiluminescence detection has been investigated. Ion-pairs of protonated tertiary amines with a chemiluminescent counter ion are on-line post-column extracted to 1,2-dichloroethane containing bis(2,4,6-trichlorophenyl)oxalate (TCPO). Hydrogen peroxide is added to the organic phase by means of a solid-state perhydrit reactor. The influence of the base catalyst (imidazole) on the chemiluminescence reaction in apolar solvents was studied. Some sulfonated chemiluminophores were compared with respect to their chemiluminescence, ion-pairing and extraction properties, and 5-dimethylaminonaphthalene-1-sulfonate was found to be the most suitable reagent. The detection limit of the potential drug secoverine is in the sub-nanogram range. |
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Keywords: | Column liquid chromatography Ion-pair extraction detection Peroxyoxalate chemiluminescence Chemiluminescent counter ion |
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