Gas Chromatographic Analysis of Volatile Sulfur Compounds from Heated Milk Using Static Headspace Sampling

An investigation was conducted to test the feasibility of using gas chromatography with static headspace sampling as an objective tool to measure milk flavor quality. Heated milk off-flavor was chosen for study. Different strategies were tried for increasing the sensitivity of a commercially available headspace method, including salting out with sodium sulfate, cryofocusing during injection, and applying backpressure to the sampling loop. With the aid of a sulfur-specific detector, the resulting system was sufficiently sensitive to detect the sulfur volatiles, H₂S and dimethyl sulfide, at the concentrations found in pasteurized skim milk. Milk that was heated to varying degrees was analyzed, and the analytical results were compared with the intensity of heated flavor as determined by a sensory panel. For skim milk, correlations were moderately strong: Spearman's correlation coefficients for H₂S and dimethyl sulfide were .75 and .60, respectively. Correlations were weak for whole milk.