The long-chain alcohol and aldehyde contents and compositions were determined in seven types of the non-centrifuged cane sugar kokuto (Kokuto A to G). Long-chain alcohols, known as policosanols, have been reported to have beneficial effects on human health. Policosanols were extracted effectively with hexane/methanol (20:1 v/v) and long-chain aldehydes were extracted with chloroform/methanol (2:1 v/v). These compounds were then analyzed by gas chromatography and gas chromatography-mass spectrometry. Trimethylsilyl ethers, the policosanol fragments, and a number of unique aldehyde fragments were analyzed to identify the source compounds. Octacosanol (C28-OH) was confirmed to be the main component in all kokuto samples. Moreover, the production process influenced the policosanol and long-chain aldehyde contents in kokuto. Kokuto A, which was produced by an open pan boiling method, showed the highest content of policosanols (86 mg/100g) and long-chain aldehydes (9 mg/100 g).