Turkish Raki is a type of traditional aniseed spirit produced in different areas of Turkey. The amounts and the repartition of the alcoholic fermentation products (fusel alcohols, esters, and aldehydes) are mainly responsible for the flavours and quality of the spirit. Previous studies have been carried out on the quantification of the volatiles of the different aniseed spirits using GC and GC-MS. In this study of 20 different commercial brands of bottled Raki and 5 homemade Turkish Raki products, the major volatiles and methanol were determined using direct injection with GC-MS. SPME extraction was also used as a confirmation method for the separation of Raki volatiles. Eight different substances were successfully identified using SPME extraction. The results indicated that some homemade Turkish Raki products from the different regions contained slightly higher concentrations of the most studied compounds. The toxic compound methanol was detected only at a level far below the acceptable legal limit.