A method of gas chromatography-mass spectrometry（GC-MS） with solid phase extraction was developed for the determination of nitrogen compounds in fluid catalytic cracking（FCC） diesel fraction.The neutral and alkaline nitrogen compounds in FCC diesel fraction were separated and concentrated by solid phase extraction（SPE） technique.The type and dosage of different elution solvents were optimized.It was found that dichloromethane and acetone-dichloromethane could effectively separate the neutral and alkaline nitrogen compounds in FCC diesel.The recovery and repeatability of the SPE method were investigated.Results showed that the recovery of the separation method was as high as 99.5%，and the relative standard deviations for the repeatability results of three separation experiments were less than 4%.The separated components were confirmed by gas chromatography-mass spectrometry（GC-MS）.It was revealed that neutral nitrogen compounds generally consisted of C0-C3 indoles and C0-C5 carbazoles，while alkaline nitrogen compouns were made up of C1-C4 anilines and C0-C2 quinolines.The quantitation on nitrogen compounds was carried out by gas chromatography with nitrogen chemiluminescence detector（GC-NCD）.Results showed that 96.6% of the identified compounds in FCC diesel attributed to the neutral compounds，in which the content of carbazoles was the highest，accounting for 64.3% of the total of the qualified nitrogen compounds.From the aspect of compound structure，the content of nitrogen compounds increased first and then decreases with the increase of the number of methyl substituents.In general，this method could be used in the analysis on the type distribution of nitrogen compounds in FCC diesel fraction.