Beer is one of the most commonly consumed alcoholic beverages, and thorough and robust analysis of the raw materials used in the brewing process, as well as the finished product, is paramount to ensure consistent product quality and taste. There are a number of potential by-products and spillover products of the beer fermentation process which can potentially negatively impact the beer’s flavors, including vicinal diketone (VDK) compounds 2,3-butanedione (diacetyl) and 2,3-pentanedione, as well as acetaldehyde. Historically, breweries use two separate GCs, or two separate analytical runs in the testing of beers - one for the analysis of VDKs, and another for the analysis of acetaldehyde, which is potentially cost-prohibitive to many breweries. In this application note, an optimized method for the simultaneous analysis of VDK and acetaldehyde in beer in presented, using a PerkinElmer Clarus® 690 GC ECD/FID with a TurboMatrix™ HS-40.