Low-level radiometric detection in LC using solvent segmentation and an effluent storage loop

Summary In this study a new approach is presented for on-line radiometric detection in reversed phase LC of medium to low polarity compounds labelled with¹⁴C. The test compounds,¹⁴C-carbaryl and¹⁴C-parathion, are extracted post-column into a non-water miscible liquid scintillation cocktail. The segmented two-phase system formed is introduced into the beta-detector without phase separation and collected in a capillary storage tube. After completion of the LC separation and detection process, the direction of the flow in the storage system is reversed and the segmented contents of the loop led at lower flow-rates through the beta-detector again. An enhanced signal, corresponding to the increase in counting time is obtained without measurable peak broadening. The lowest possible detection limit of the system is 9 counts per peak corresponding to subnanogram quantities of tested pesticides. Calibration curves are linear over at least 2 orders of magnitude and have the expected theoretical slopes. The reproducibility of the system is better than 4 % rel. S.D. An application to a recovery study of parathion shows the practical potential of this technique. Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984