Optimization of Flame-Based Sulfur Chemiluminescence Detection (SCD) with Microcolumn High-Performance Reversed-Phase Liquid Chromatography

Through a detailed optimization process, response surfaces were obtained for micro-HPLC/SCD under various reversed-phase (methanol/water) elution conditions. Linear dynamic range, correlation coefficient, response factor, and limit of detection were found to vary with mobile-phase composition. The lowest sensitivity achieved was a detectivity of 600 fg of S/s at a mobile-phase composition of 40% methanol/60% water. Application of the HPLC/SCD interface to the separation of thiocarbamates extracted from apples is presented