It is important to determine regulated heavy metals such as cadmium, lead, and uranium, whose concentrations are extremely low in the environmental samples. Solid-phase-extraction is one of the effective techniques that could preconcentrate target heavy metals and separate them from the interfering elements. AIST developed a hybrid solid-phase-extraction method (Fig. (a)), in which the sample loading to the syringe-driven column was performed off-line while the elution and measurement of heavy metals were performed on-line. This method integrated the capabilities of multi-sample pretreatment and highly-sensitive measurement, which are the typical merits of off-line method and on-line method, respectively. Figure (b) shows that an off-line method (violet line) and the hybrid method (red line) respectively provided approximately 3-fold and 10-fold (commercial columns) enriched signal intensities compared to that of none-preconcentrated sample (green line). It is noted that the newly developed column could improve the enrichment factor up to approximately 65-fold.