title: Multivariate optimization of headspace trap for furan and furfural simultaneous determination in sponge cake.
abstract: Furan, a possibly carcinogenic compound to humans, and furfural, a naturally occurring volatile contributing to aroma, can be both found in thermally treated foods. These process-induced compounds, formed by close reaction pathways, play an important role as markers of food safety and quality. A method capable of simultaneously quantifying both molecules is thus highly relevant for developing mitigation strategies and preserving the sensory properties of food at the same time. We have developed a unique reliable and sensitive headspace trap (HS trap) extraction method coupled to GC-MS for the simultaneous quantification of furan and furfural in a solid processed food (sponge cake). HS Trap extraction has been optimized using an optimal design of experiments (O-DOE) approach, considering four instrumental and two sample preparation variables, as well as a blocking factor identified during preliminary assays. Multicriteria and multiple response optimization was performed based on a desirability function, yielding the following conditions: thermostatting temperature, 65°C; thermostatting time, 15min; number of pressurization cycles, 4; dry purge time, 0.9min; water / sample amount ratio (dry basis), 16; and total amount (water + sample amount, dry basis), 10g. The performances of the optimized method were also assessed: repeatability (RSD: ≤3.3% for furan and ≤2.6% for furfural), intermediate precision (RSD: 4.0% for furan and 4.3% for furfural), linearity (R2: 0.9957 for furan and 0.9996 for furfural), LOD (0.50ngfurangsample dry basis-1and 10.2ngfurfuralgsample dry basis-1), LOQ (0.99ngfurangsample dry basis-1and 41.1ngfurfuralgsample dry basis-1). Matrix effect was observed mainly for furan. Finally, the optimized method was applied to other sponge cakes with different matrix characteristics and levels of analytes.
authors.affiliation: UMR Ingénierie Procédés Aliments, AgroParisTech, Inra, Université Paris-Saclay, 91300 Massy, France.
authors.forename: Mayela
authors.initials: M
authors.lastname: Cepeda-Vázquez
authors.affiliation: UMR Ingénierie Procédés Aliments, AgroParisTech, Inra, Université Paris-Saclay, 91300 Massy, France.
authors.forename: David
authors.initials: D
authors.lastname: Blumenthal
authors.affiliation: UMR Ingénierie Procédés Aliments, AgroParisTech, Inra, Université Paris-Saclay, 91300 Massy, France.
authors.forename: Valérie
authors.initials: V
authors.lastname: Camel
authors.affiliation: UMR Ingénierie Procédés Aliments, AgroParisTech, Inra, Université Paris-Saclay, 91300 Massy, France. Electronic address: barbara.rega@agroparistech.fr.
authors.forename: Barbara
authors.initials: B
authors.lastname: Rega
mesh_terms: D005504:Food Analysis; D005506:Food Contamination / Q000032:analysis*; D005662:Furaldehyde / Q000032:analysis* / Q000302:isolation & purification*; D005663:Furans / Q000032:analysis* / Q000302:isolation & purification*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D015233:Models, Statistical; D015999:Multivariate Analysis; D015203:Reproducibility of Results
chemical_list: D005663:Furans; D005662:Furaldehyde; C039281:furan
keywords: Desirability function; Optimal design of experiments; Random blocks; Response surface; Stable isotope dilution assay; Standard addition method