An adaptation is presented of method 8261--from the Office of Solid Waste and Emergency Response Test Methods for Evaluating Solid Waste Physical/Chemical Methods (SW-846)-to analyze milk for an expanded list of volatile organic compounds is presented. The milk matrix exhibits a strong affinity for organic compounds and the surrogate based matrix normalization described in method 8261 provided accurate results. This method had the sensitivity necessary to detect volatile organic analytes at or below maximum contaminant levels (MCLs) set by EPA for drinking water. In a survey of milk samples available in Las Vegas, Nevada, 32 of 88 targeted volatile organic compounds (VOCs) were detected. Many of the detected VOCs have not previously been reported and a rationale for their presence in milk is presented.