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To overcome the peak band broadening and to increase the peak capacity and separation efficiency of a two-dimensional liquid chromatographic system, a high-temperature normal phase liquid chromatography (HTNPLC) was used as the first dimension (lst-D), and a RPLC was used as the second dimension (2nd-D). The sample was first separated on the lst-D CN column and the primary eluent stored in the sampling-loop system alteatively (in HTNPLC × RPLC mode) or selectively (in HTNPLC/RPLC mode) and was then transferred to 2nd-D C18 column for further separation. The resolution and separation efficiency of the systems were greatly improved. The systems were evaluated by analyzing several polycyclic aromatic hydrocarbons and Glycyrrhiza uralensis extract.