Randomized blocked design applied for the multicriteria optimization of headspace trap extraction of furan and furfural from sponge cake

Furan, a possibly carcinogenic compound to humans, and furfural, a naturally occurring aroma compound, can be produced in heat - processed foods [1,2]. Therefore, their simultaneous determination is important for food safety and quality purposes. Headspace techniques coupled to gas chromatography - mass spectro metr y (G C - M S ) are often used to analyze process - induced compounds. Although headspace trap (H S Trap) extraction has been recently used for furan quantitation in bread crust [3], this technique has not been used for the simultaneous determination of furan and furfural before. This work presents an optimal design of experiments ( O - D O E) approach using random blocks for the multicriteria optimization of H S Trap extraction of furan and furfural from sponge cake for their quantification by G C - M S . A bias related to sample preservation was observed during preliminary tests and eliminated in further assays by considering it as a blocking factor. A tailor - made experimental plan including four instrumental factors (i.e. thermostatting temperature and time, dry purge time, pressurization cycles) and two sample preparation variables (i.e. ratio of water and sample weight [dry basis] and total amount [dry basis]), considering the blocking factor was designed. Response surface models ( P - value <0.0001; R 2 0.974 for a ll mode ls) resulted in the identification o f most linear and so me quadratic terms and a few second order interactions as influencing the extraction of furan, furfural and their internal standards, d4 - furan and d4 - furfura l. Interestingly, one of the samp e preparation variables, namely the ratio of water and samp le weight (dry basis), showed no effect on furfural extraction, while different profiles for furan and d4 - furan were observed regarding this factor. A set of optimal conditions for a H S Trap extraction method was, for the first time, success fully defined by using the optima design of experiments methodology and a desirability function.