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The heavy oils from petrochemical industry were analyzed by an on|line coupled packed capillary high performance liquid chromatography(%μ%|HPLC) and high temperature capillary gas chromatograph(HTGC). An aminosilane silica packed %μ%|HPLC column separates the sample into aliphatics, one|to five|ring polycyclic aromatic hydrocarbons and resin ect.. The volume of each fraction is about 30~60 μL, which is stored in turn in a multi|loop interface from a single LC injection, and then transfered into GC for quantitative analysis. The content and the carbon number distribution of each chemical class are obtained. The RSD is less than 5%. Examples were given to demonstrate the applicability of the method.