Book excerpt: A headspace SPDE-GC/MS method for the analysis of the volatile fraction of beer was developed and optimized. The optimization step was carried out using two level full factorial and Doehlert designs for the determination of the optimum extraction conditions, and the optimized method was used for the analysis of five commercial beers, and a variety of compounds from different chemical classes were extracted from each sample, reflecting the difference in volatile profile among beers brewed with different raw materials, adjuncts, and brewing conditions.