Characterization and Semiquantitative Analysis of Volatile Compounds in Orange Juice by Use of Headspace-Solvent Microextraction and Gas Chromatography

By alternate use of two different extraction solvents, n-hexadecane and benzyl alcohol, a headspace-solvent microextraction (HSME)–GC–FID/MS method has been established for characterization of the volatile components of an orange juice beverage. The method avoids two disadvantages of conventional HSME—difficulty identifying components obscured by the solvent peak and inefficient extraction of some of the compounds if one solvent only is used. The optimum conditions (droplet volume, equilibration temperature and time, extraction time, and ionic strength) were determined by the factor-rotation method. The volatile components of the beverage were mainly terpenes, terpenols, fatty acids, and alcohols, for example limonene (114.71 mg L⁻¹), phellandrene (4.50 mg L⁻¹), terpineol (p-menth-1-en-8-ol; 3.12 mg L⁻¹), α-pinene (0.33 mg L⁻¹), n-hexadecanoic acid (0.28 mg L⁻¹), and terpinol (0.13 mg L⁻¹).