A mixture of [H]-geraniol, [H ]-nerol, [H]-linalool and [ H]-α-terpineol was prepared for use as internal standards in a rapid and accurate analytical method, employing gas chromatography-mass spectrometry (GC/MS), to determine the concentration of geraniol, nerol, linalool and α-terpineol in wine. The method avoids the possible formation, degradation and interconversion of these compounds during their analysis.