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A capillary column was prepared by continuously packing ostadecylsilane (ODS) and taurine derivatized silica (TDS) in one column without interface. This continuously packing chromatography (CPC) column is easy to operate, has good stability and shows simultaneously separation of both polar and non-polar compounds. The simultaneous separation of a series of complex samples with highly hydrophobic components (benzene, toluene, ethylbenzene, and PAHs) and highly hydrophilic components (biogenic amines, bases and nucleosides) using this CPC method was investigated. The relative parameters such as the volume fraction of acetonitrile and length of the ODS and the TDS phases were investigated and optimized. The experimental results show that this column combines the advantages of both ODS and TDS stationary phases, and exhibits a reversed phase liquid chromatography (RPLC) mode followed by a hydrophilic interaction liquid chromatography (HILIC) mode when 80% of acetonitrile was used in the mobile phase. The satisfactory results indicate that the CPC method provides an easy way to simultaneously separate polar and non-polar compounds.