Development of a headspace solid-phase microextraction gas chromatography mass spectrometry method for the quantification of volatiles associated with lipid oxidation in whole milk powder using response surface methodology.

• 13 compounds derived from lipid oxidation were quantified by HS SPME GC–MS. • A central composite rotatable design was used to optimize HS-SPME parameters. • Response surface methodology assessed the effects of extraction parameters. • Method validation included LOD, LOQ, and precision. Lipid oxidation is a major contributor to the deterioration of the sensory quality of fat-containing dairy powders. Hydroperoxides are the primary oxidation products from unsaturated fatty-acids that readily yield a complex mixture of volatile organic compounds that can adversely impact product quality and shelf life. Headspace solid-phase microextraction gas-chromatography mass-spectrometry was chosen to quantify thirteen lipid oxidation compounds in whole milk powder encompassing a range of volatilities and chemical classes. A central composite rotatable design (CCD, α = 1.1) based on a 23 factorial table was used with response surface methodology to optimize the HS-SPME parameters; determined at; 45 min extraction time and 43 °C extraction temperature. The significant model terms were found to be extraction temperature (p < 0.05) and the interaction between time and temperature (p < 0.05). Precision, accuracy, LOD and LOQ were determined and the method was validated for whole milk powder. [ABSTRACT FROM AUTHOR]