Shark liver oil is an important functional oil， which is rich in functional factors such as squalene and shark liver alcohol， and has good physiological activity. The aim of this study was to study the changes of volatile components in the refining process of shark liver oil. A new laser-assisted headspace solid phase microextraction combined with mass spectrometry （LID HS-SPME-GC/MS） technique was used to rapidly analyze the volatile components of crude shark liver oil during degumming， acidification， decolorization and deodorization. The results showed that the content of undesirable volatile compounds reduced significantly during refining process（P < 0.05）. Among them， the change of nonanal content was the most significant. Compared with crude shark liver oil， the content of nonanal was reduced by 20.46%， 37.24%， 61.84%， and 95.66% respectively after degumming， acidification， decolorization and deodorization. Six important characteristic flavor substances， namely 2-undecone， 1 -penten-3-ol， furfural， 2-nonanone， hexanal， octanal were determined by principal component analysis （PCA） and orthogonal partial least-square discriminant analysis （OPLS-DA）. This study can provide a theoretical basis for refining process to effectively improve the composition of volatile substances in crude oil.